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All 244 posts   Subject: Success making GBL!   Please login to post   Down

 
    Chromic
(Synaptic Self-Mutilator)
01-01-03 03:46
No 394630
      Success making GBL!
(Rated as: excellent)
    

We are now this (><) close to a writeup, as I've finally got a procedure that works very well! Here's the procedure:

Mixed 0.355mol GABA (36.6g), 0.300L water & 0.355mol sodium nitrite (24.5g) in a 1L flask sitting in an ice-bath (vented fumes to the outside, as poisonous nitric oxide is produced). Very, very slowly added 0.178mol 33% sulfuric acid (17.8g 98% H2SO4 with 2 parts water) using a pressure-equalized addition funnel. Let run for 7p-2p (should have let run longer, ie 36hrs... but was in a hurry for the new year! the yields will most definitely go up if you do allow it to run longer...)

Then 0.38mol NaHCO3 (~32g) was added and refluxed for 30 mins, then reduced to half volume (~150ml) by simple distillation. 0.355 mol H2SO4 (35.5g) was added. Extracted with 4x100ml of DCM. Distilled off DCM (38-190C), then GBL (at 198-202C) to recover 15.8g of GBL. 57% yield!!!

AT LAST... SUCCESS! smile The bioassay is, without a doubt, ABSOLUTELY POSITIVE! The quality is the same as A.C.S. butyrolactone.

Thank you fierceness & the hive in general!

References:
Post 371855 (fierceness: "GABA -> GHB", Chemistry Discourse)
Post 364034 (Chromic: "msg -> ghb?", Chemistry Discourse)
 
 
 
 
    moo
(Hive Bee)
01-01-03 07:07
No 394658
      Congratulations     

Way to go!
 
 
 
 
    pHarmacist
(Hive Addict)
01-02-03 01:08
No 394764
User Picture 
      Chromic     

Excellent pioneer reasearch work!

"Turn on, Tune in and Drop Out"
 
 
 
 
    Semtexium
(Hive Elder)
01-02-03 13:24
No 394837
      :-)     

smile

crazylaughsmiletonguewink    Mean People Suck    winktonguesmilelaughcrazy
 
 
 
 
    gabd
(Hive Bee)
01-02-03 19:53
No 394897
      And how much is a dose     

Since it always comes diluted and ready to serve over here(not as the sodium salt) I was wondering what was the dose you felt was good?
I'm just wondering before trying this.
Thanks for the write up Chromic!
 
 
 
 
    pHarmacist
(Hive Addict)
01-03-03 04:05
No 395021
User Picture 
      Chromic     

Distilled off DCM (38-190C), then GBL (at 198-202C) to recover 15.8g of GBL. 57% yield!!!

So there were no more than 2 fractions; solvent and GBL, nothing else? In other words; Was there anything remaining in the distillation flask?

"Turn on, Tune in and Drop Out"
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-03-03 09:21
No 395078
      Dosing     

2ml is a good starter dose for guys, 1.5ml for girls. 2.8ml is my usual dose, but I've built a good tolerance / brain damage resulting from the stuff. This stuff doses like pure GBL.

Btw, I spoke too soon about the purity. There is a weird, intense sour taste to the GBL. I've got no idea what it is? Perhaps converting to NaGHB before ingesting the product would be a good idea...

A black crap remains in the distilling flask, indicating that solvent extraction, by itself, does not give a product that is suitable for human ingestion.

... so close to a write up ...
 
 
 
 
    hCiLdOdUeDn
(Hive Bee)
01-04-03 00:40
No 395228
User Picture 
      Excellent!     

Excellent, excellent, excellent!!! Time to make me some G!

Sink or SWIM
 
 
 
 
    fierceness
(Hive Bee)
01-04-03 01:33
No 395237
      Excellent!!     

SWIF has had similar results as well with his last run.  However, DCM is very difficuly to obtain here; will a NP solvent like Xylene/Toulene work equally as well?  Perhaps swif will try to use one of these solvents and see.

Great Work!
 
 
 
 
    fierceness
(Hive Bee)
01-04-03 02:30
No 395242
      DCM/GBL separation.     

Instead of having to go through the distillation drama, could one separate the final GBL/DCM mixture via titration with NaOH?  Keep adding NaOH/water to the DCM until the pH of the water is about 8, then add vinegar to decrease the pH back to 7.

Just a suggestion
 
 
 
 
    fierceness
(Hive Bee)
01-04-03 02:40
No 395245
      Prelim. Writeup: GABA -> GBL     

GABA to GBL writeup
**this writup is only preliminary, and mainly is to facilitate perfection of this method **




Introduction:

First of all, MANY MANY thanks to Chromic for helping to pioneer this method.  This is simply without a doubt one of the easiest methods to make GBL for the clandestine chemist.  Through some trial and much error, respectable yields finally have been obtained.




Chemicals (in relation/ratio to the main precursor, GABA):

1 part Powdered GABA   ( ***  Do *NOT* use @NC brand GABA.  Although many nutritional stores claim there are no adulterants, there most definitely are. )

0.68 part Sodium Nitr[bold]ite[/bold]  (*** NOT NITRATE)

0.5 part conc H2SO4

(in other words, GABA:Sodium Nitrite:H2SO4   1:0.68:0.5)

ACS NaOH or Baking Soda   ( ** if you cannot get ACS NaOH, USE BAKING SODA

DCM (possibly other solvent, let us know if any others work!)






Procedure:

1. Dissolve GABA and Sodium Nitrite in a flash with water in an ice bath.

2. Make a mixture of 1 part conc H2SO4 2 parts water.

3. Put this mixture in a bottle capable of dripping VERY slowly (swif uses those red and yellow plastic ketchup and mustard bottles).

4. With stirring/swirling, let the H2SO4/water mixture drips very slowly into the GABA/NaNO2 mixture until all of it is used up.  **IF YOU SEE BROWN GASSES, YOU ARE GOING TOO FAST -- THESE GASSES ARE POISONOUS **

5. Put the flask outside or somehow vent it outside as some of the gasses emitted are also poisonous and let sit for at least a day, 2 is preferable.  You should see little bubbles of N2 being formed in the flask.

6. Now you need to convert all of the GHB/GBL into NaGHB so we can boil off all of the liquid.  The GBL will steam distill, so that is why we convert it to NaGHB.  You can add about 0.90 parts (compared to the original GABA) baking soda and reflux for 30 minutes to an hour.  Alternatively, (swif's method of choice) you can use ACS NaOH (not lye) until the pH is neutral (7-8, a little more basic than neutral is OK).

7. Boil off about half of the solvent and add 1 part H2SO4.  This is to destroy any dangerous nitrosamines and to convert the NaGHB back to GBL.

8. Extract the GBL with DCM ( uncertain if any other solvents will work, eg toulene, xylene) two or three times and combine the extracts.

9. Now you must separate the DCM from the GBL.  One easy way of doing this is to prepare a boiling water bath and place the flask in there.  The DCM will boil away, but the GBL will remain since its boiling point is much higher.  *NOTE*

10. What you have left is GBL and some impurities.  You can distill out the GBL at 200 deg. celcius.  (Obviously, you cannot use the water bath ;) )  *NOTE*

11. Congratulations!  You have successfully made GBL.  You can consume as-is, or convert to to Na/K GHB.  An active dose is 1-2mL of GBL.  GBL is a harsh mucous membrane irritant; be sure to dilute it in something! Enjoy!

*NOTE*  There is another hypothetical method of separation that has not been tested yet.  If it works, let us know!  Titrate the DCM/GBL mixture with 50% NaOH and when the water is pH 8 or so, separate the water, and add enough vinegar until it is pH7 again.

Again, many thanks to Chromic and the hive in general for all the help in helping to formulate this procedure!
 
 
 
 
    Anansi
(Hive Bee)
01-04-03 03:37
No 395253
      A minor point - ingestion of lactones.     

I am fully aware that this has been stated quite clearly in previous posts at the hive, but as it's not mentioned in fiereness' preliminary writeup or since somebody asked about dosages in this thread I'll mention it again -

lactones eat mucus membranes - this includes the lining of your throat and nasal passages. Thus GBL MUST be diluted in a substancial volume of water before it is consumed or it will do quite some damage on the way down!!

I don't know from PERSONAL experience what a suitable dilution it, but suggestions as to what level of dilution is appropriate are plentiful here, just UTSE.

This thread outlines a very accessible and relatively simple route to GBL, and it likely to be attempted by people with less than the desirable level of chemistry/safety knowledge. Just wanted to add the warning regarding lactone ingestion to the other safety information (NOx toxicity/nitrosamine toxicity etc) already contained herein.

...Anansi
 
 
 
 
    fierceness
(Hive Bee)
01-04-03 03:43
No 395260
      edited to reflect as such.. thanks!     

edited to reflect as such.. thanks!
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-04-03 07:30
No 395306
      On ingesting and cleaning up     

1ml GBL / 20ml aqueous is the absolute minimum dilution to make pure GBL safe to the body. I would recommend something closer to 1ml / >50ml orange juice. I'm positive that distilling off the solvents and then using as is, is simply not good enough to reach the proper purity (distilling with water, then reacting with base is definitely a better way to go). I've done it, and you get a nasty brown aweful smelling liquid.

I'll let you guys know of my next run, which I hope pushes the purity far enough to drink. I really do wonder what that nasty smell is (perhaps I just needed to add a few ml of water once the DCM boiled off to take away that smell...) I wish I had a GCMS. smile I'd also love to hear of solvents that would have a greater affinity for GBL than DCM (perhaps ethyl acetate?).
 
 
 
 
    SPISSHAK
01-04-03 08:08
      tetrahydrofuran
(Rated as: insignificant)
    
 
 
 
    fierceness
(Hive Bee)
01-04-03 19:10
No 395424
      What about taking the DCM/GBL mixture and...     

What about taking the DCM/GBL mixture and titrating it with NaOH and separating the two layers like the last step of an A/B?   Would that effect a reaction between the NaOH and the GBL to form NaGHB and move it into the water layer?
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-04-03 23:53
No 395467
      Good idea!     

Good idea! I think I'm going to go ahead with the same method as I proposed, but why not give that a try for your next run? Perhaps the crap would stay in the DCM... and perhaps not, but who knows...
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-05-03 07:24
No 395540
      More details     

.355mol GABA, standard procedure (but used the right amount of HCl instead, then added 25% excess HCl 16hr later and worked up 8hrs after that). 1.5 eq baking soda, refluxed. Distilled off half volume, 1.2 eq H2SO4. Extracted 4x100ml. Distilled 23.1g GBL (196-204C). 76% yield. The GBL tastes fucking AWEFUL. I really appologize about this, I shouldn't have started a new thread until I had a procedure that worked well.

I'm going to convert to NaGHB and hope for the best. Fuck.
 
 
 
 
    fierceness
(Hive Bee)
01-05-03 07:48
No 395543
      appropriate solvent for GBL :)     

swif has no DCM.. suggestions for other solvents for GBL by anyone would be greatly appreciated :) toulene? xylene? ether?  swif may try toulene and see what happens..

GBL is soluble in water, so I can't do a water wash of the toulene before adding base..  will try it in the next run.. any other suggested (preferably otc) solvents would be greatly appreciated :)
 
 
 
 
    pHarmacist
(Hive Addict)
01-05-03 08:56
No 395547
User Picture 
      ether     

Et2O would be ideal for the extraction! You can use toluene as GBL seems to have a rather high B.P. That if you don't have Et2O.

Accept No Imitations, There Can Only Be One; www.the-hive.ws
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
01-06-03 03:49
No 395682
User Picture 
      sounds better than THF as starting material..     

  I know that purchasing this stuff from a chem co. wouldn't be suspicious, but how much$$$$ does GABA go for? Seems like any decent co. could special order it if they don't have it. No haz-mat fee, so it's probably a cheaper starting material than THF..

Love my country, fear my government.
 
 
 
 
    fierceness
(Hive Bee)
01-06-03 04:42
No 395706
      It is definately better.     

It is definately better.  Do a quick google search for it.  You'll get a number of hits.
 
 
 
 
    hCiLdOdUeDn
(Hive Bee)
01-06-03 23:38
No 395931
User Picture 
      Price to make GBL     

Using a quick Google search...

GABA costs $15 per 100g
Sodium Nitrite costs $5 per 100g

Using Chromics amounts & yields a Bee could make 100g of GBL at a cost of $42.46 for just GABA and Sodium Nitrite. This is of course more if you dont have basic chemicals and equipment e.g. Baking Soda, Sulfuric acid, glassware, etc.

If a dose of GBL is 2g then it would cost about 85 cents per dose. 

If yields are 100% then expect costs to decrease by half.

Sink or SWIM
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-07-03 04:59
No 396023
      <nod>     

Why else would I pursue a route unless it was in some way practical? smile THF was something that I tried time & time again to get it to work with nothing but violent or noxious failures.

$60/kg for GABA, $9/kg for 700g nitrite. That should yield about 650g GBL (according to my latest yield), or about 325 good-sized doses, which is $0.20/dose. I suppose you need to tack on shipping and handling and the cost of baking soda and drain cleaner, but even still, the cost should not ever go above $0.20/g.

The trouble still remains in removing the contaminents. Neutralizing with baking soda and then boiling down does not give a suitable product. It has a very off flavor that makes one want to puke when tasted (not very noticeable when smelled). Sure, it seems to get me high--but at what cost? (am I to develop cancer in the next year? ... ugh)

I've increased the scale yet again (to 0.5 mol) and should have some better, more meaningful yields to share. I'm still at a loss on purifying it, which prevents me from releasing a write up.
 
 
 
 
    placebo
(not quite as irritable lately)
01-07-03 06:19
No 396043
User Picture 
      BDO to GBL is nice and easy via the copper...     

BDO to GBL is nice and easy via the copper chromite catalyst and at 200L of BDO for about US$1000  and the cat costs about US$20, is nice and cheap at 16c/mL. But as BDO is getting too hard to aquire, this could be the next best bet assuming we can get a nice cleanup method. Chromic, you were saying you have distilled the GBL or are you just distilling off the DCM and then made up the remaining GBL into GHB? Anybody have a mail-order source for GABA I can use so I can try this? I tried my local health food shope and they have no idea...

The other thing that I was thinking about is GVL as it is not scheduled here or the US as far as I can tell. and 18% stronger! I may see if I can order it.

Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)
 
 
 
 
    carcrash
(Hive Bee)
01-07-03 10:12
No 396088
      Clean up of final product     

After distilling what about freezing slowly in the refridgerator to force out impurities? Doubling the volume with water after you pull the dcm off may let you steam distill out the sour taste. As far as the sour taste did you check the ph afterwords by adding a bit to distilled water? Wondering if you didnt neutralize all the acid. I have also read on the hive about people noticing a difference in E that was gassed with hcl into sulfuric. Somehow a trace of the sulfuric carried over. Maybe a small amount of activated carbon would get rid of some of the impurities during distillation. If you distilled till dry or even close to it some of the residue may have burned. A small amount of safflower oil might let you distill off all the gbl and trap the residue vapors and or contaminents in the final product.

GBL
Melting point­ 43
Boiling range 201-206
Flash point 104

Not a chemist I just follow directions on the box mix
 
 
 
 
    Chimimanie
(Newbee)
01-07-03 15:39
No 396148
User Picture 
      GVL or GHV     

GVL or Na-GHV are ineffective as GHB substitute. I have bought some pure GVL to test them and even at 10g of the NaGHV or 8 ml of the GVL I couldn't notice any effect (but the first time I tried it I got a (placebo) response (for 15-20 min) like when I was on a butanediol binge for 4 days when the food become sweet and the colors more colorful, some hours before the harsh withdrawal begin.)

Anyway I used more than 1000 dose of ghb/1,4 butanediol when I could buy it no problem and an effective dose for me is about 2.8-3.4 ml of 1,4 with 4 ml or more is a temporary coma. I conclude than GHV/GVL don't substitue at all and that they do not have any effect. Its only waste of money.

Maybe the T-HCA (trans-4-hydroxy-crotonic acid) is effective? I dunno, haven't tested it...
 
 
 
 
    El_Zorro
(Hive Addict)
01-07-03 21:30
No 396221
      Chromic- Have you tried titrating the GBL...     

Chromic-

Have you tried titrating the GBL mixture to GHB, and then doing a NP wash on it?  Wouldn't that take care of a lot of the impurities?  Then it could be converted back to GBL and distilled, no?

It is seductive, way too seductive.             -Eleusis
 
 
 
 
    StraightEdge
(Hive Bee)
01-07-03 21:48
No 396227
      a suggestion     

I know this would barely do anything, but I think you should try converting to NaGHB then boiling down to the solid form. That might be a good way of double-checking the yields, at least. Although I don't know shit about chemistry, it seems to me that distilling would leave you with only liquid impurities at worst. If that is the case, then an attempt to solidify would leave you with a goopy mess rather than the dry solid. That is, unless the impurity has the same/similar melting point as NaGHB. If you do get a solid product, it may be a good idea to check the melting point, just to be sure. That or you could try what car crash said, putting in some activated charcoal. The problem is that it could absorb some of the GHB or GBL. Or maybe it wouldn't, I am not very familiar with the properties of activated charcoal. Filtering out the charcoal is a hassle as well, because a coffee filter is too coarse to do an effective job. I guess you could distill after mixing with charcoal, but there is no guarantee that the impurity would bond to the charcoal.

Did the GBL taste that bad in your initial dream (the one in the first post)?
 
 
 
 
    fierceness
(Hive Bee)
01-07-03 22:49
No 396250
      Fork in the road.     

placebo: SWIF has done a regular water distillation of the post-rxn contents and thrown away the initial forerun and the nasty sour taste that Chromic is talking about still persists.  Also, GVL has the sedative properties but not the euphoric proprerties of GBL/GHB. 

Chromic (or anyone else with an idea): Swif has a flask of post rxn contents now; what method should he attempt to use in purification?  Should he add a mol eq. of H2SO4 and attempt to extract with Toulene, and then titrate the toulene with NaOH and separate the layers to get NaGHB in solution? 
 
 
 
 
    El_Zorro
(Hive Addict)
01-08-03 01:14
No 396296
      Try titrating the mixture with NaOH, then...     

Try titrating the mixture with NaOH, then doing a NP wash.  Then add the molar eq. of H2SO4, and then extract with NP, and distill.  Maybe that'll work, who knows.

It is seductive, way too seductive.             -Eleusis
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-08-03 03:27
No 396331
      gaba -> ghb     

I've got the 0.5mol rxn done right now, my current idea is to reduce the volume as far as I can (perhaps 200ml). Pour off the liquid (inorganic salts normally crash out), then acidify. I'm going to keep my fingers crossed and hope for the best.

I'd really recommend trying to reduce the volume before you extract with toluene, this way you increase the concentration of salt and decrease the concentration of water pushing more of the GBL out of solution. I'm not sure if using toluene is the best idea (I hope you have some good distillation equipment, as I would have to recommend that you distill the GBL before drinking it!), but GBL is soluble in it.
 
 
 
 
    fierceness
(Hive Bee)
01-08-03 04:53
No 396342
      Re: I'd really recommend trying to reduce the...     



I'd really recommend trying to reduce the volume before you extract with toluene, this way you increase the concentration of salt and decrease the concentration of water pushing more of the GBL out of solution. I'm not sure if using toluene is the best idea (I hope you have some good distillation equipment, as I would have to recommend that you distill the GBL before drinking it!), but GBL is soluble in it




I was just giving a possible suggestion.  What about a water/steam distillation (after adding a molar eq of h2so4)followed by a basing out of the salt forming NaGHB + extra NaOH.  Then boil off all the liquid which should leave us with NaGHB plus maybe some NaOH -- it should remove the volatile impurities that came over with the steam.  Then maybe an acetone wash? or a NP wash? or recrystallazation?  I'm at a loss at that point.  I think swif will go ahead and water-distill his post rxn contents and check back here later to see what you guys suggest.

 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-08-03 05:32
No 396346
      0.5mol run     

I used too little NP this time.

0.5mol GABA, 0.5mol HCl, 0.45L water. Reacted about 24hr, added 10% excess HCl. Added baking soda, refluxed, distilled off to half volume, 1 eq H2SO4. Extracted 5x100ml. 26.3g GBL after distillation. 61% yield. N.B.: use more solvent next time!

Some of the GBL will be converted to NaGHB and I'll write more on this later.
 
 
 
 
    fierceness
(Hive Bee)
01-08-03 18:52
No 396437
      and the purity of the GBL?     

and the purity of the GBL?  How did you distill -- did you just distill off the DCM and you were left with GBL? or did you distill off DCM, then distill GBL?
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-08-03 19:59
No 396451
      GBL purity     

>and the purity of the GBL?  How did you distill

Huh? I don't understand your question. I'll explain in detail.

I distilled off the DCM in a 500ml roundbottom flask on a steaming water bath (I used a coil condenser to condense the vapors and ran it quite fast, the DCM pours over), a glass bend and a 1.5" egg stir bar. When that was done, I transferred it to a 100ml flatbottom flask (washing out with a bit of DCM), a 75mm column, 1" hex stirbar, a 3-way still head with a 400C mercury thermometer. I distilled off all of the DCM (up to 60C vapor temp, I believe). Then I replaced the condenser with a liebig condenser and just added a touch of water in the end (not circulating). Then I insulated it all with glass wool and turned the heat to max (with stirring, as all previous distillations were done). I tossed out everything that came across until I hit about 195C. I kept everything that boiled at ~197-~204C.

I took that and reacted it with NaHCO3. It turned out with the right pH and a better taste. I boiled that down to dryness, then rediluted based on the weight of the NaGHB. It's still not perfect, but I think it's safe to consume and I might release a writeup based on this.

>or did you distill off DCM, then distill GBL?

Yes, that's what I did. If you do not distill the GBL you will be left with an orangish-yellow dirty liquid. Solvent extraction, by itself, does not purify it enough to drink.
 
 
 
 
    carcrash
(Hive Bee)
01-08-03 22:12
No 396483
      Seriously try freezing it in the refridgerator     

I have a strong intuitive guess that the impurities will be forced out of the gbl. Post distillation.

Not a chemist I just follow directions on the box mix
 
 
 
 
    fierceness
(Hive Bee)
01-11-03 03:00
No 397125
      Grrrr     

SWIF ran a .5mol rxn.  For the workup, he basified, reduced volume, added 1 eq H2SO4, extracted 4x with Xylene, added a 40% NaOH solution.  BAM.  A NASTY white emulsion forms.  He is going to let it sit overnight and pray that it clears up; if not, its back to square one.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-11-03 06:45
No 397176
      Why?     

Just distill off the xylene to get the NaGHB. As so long as you didn't use a ridiculous amount of NaOH, you should be able to recover something.

I really hope that you weren't trying to extract the NaGHB without first purifying the γ-butyrolactone!!! (solvent extraction is not a good enough purification...)

Well damn it all! α-methylphenethylamines! I said it! I said it! And β-lactams! Ok, ok. I won't use any more Greek letters (as to not upset Lili).
 
 
 
 
    fierceness
(Hive Bee)
01-11-03 09:08
No 397194
      Re: I really hope that you weren't trying to...     



I really hope that you weren't trying to extract the NaGHB without first purifying the г-butyrolactone!!! (solvent extraction is not a good enough purification...)



I was hoping that maybe the impurities would stay in the NP layer.  I have a feeling, though, that is it those impurities that are causing the emulsion.  Scratch that one off the list.  Next time, swif is going to try to water/steam distill the rxn contents and then extract the distillate with a NP (after first reducing the volume) and see  what that looks like.

 
 
 
 
    Prdy2GO
(Hive Bee)
01-29-03 14:28
No 402337
      What no Sodium Nitrite?     

Was the Sodium Nitrite omitted from the writeup or is it not nessary? Please explan. I have drempt a 10mol reaction in 12hr run time with H2so4 extracted with DCM and vacuum distilled. Product was good low yeald but only extracted once with 250mlDCM will finish off the rest later just too imoacent I guess. So if the Nitrite is not needed it would be nice I am only interested in GBL for depotting or epoxy removal.

WTF is that smell... It keeps following me.
 
 
 
 
    fierceness
(Hive Bee)
01-29-03 22:11
No 402433
      the sodium nitrite is necessary..     

the sodium nitrite is necessary.. you only used 250mL of DCM to extract a 10mol run?
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
01-30-03 04:34
No 402553
      nitirite necessary     

the nitrite is necessary--how was the GBL? it's always been a really sour off-taste for me. I've been kind of scared to know what exactly I was ingesting. 10mol run? Damn!
 
 
 
 
    fierceness
(Hive Bee)
01-30-03 04:53
No 402561
      i wish someone with access to the right ...     

i wish someone with access to the right equipment would try this out and let us know <nudge>
 
 
 
 
    M3Psych
(Stranger)
01-31-03 00:04
No 402801
      ascorbic acid     

It is well known that sodium ascorbate or ascorbic acid prevent the formation of nitrosamines (in vitro and in vivo). Would this be of use? Could it be added to the synth without screwing up the rxn?

Aside from left-over solvent, unreacted H2SO4 (etc), the nitrosamines would be the only toxic compounds in this rxn so if ascorbic acid can be used the product after distillation should be nearly as pure as any (probably at least 99.8%). Filtering with activated charcoal should be adequate to bring it up to 99.9%. You could even re-distill after this filtration and see if the taste is gone. It should be if the pH is properly adjusted.

You'll lose probably 10% from the charcoal filtration but it's a small price to pay for a pure product. SWIM's first GBL experience was with 99.8% pure GBL. It was dizzying and unpleasant. After extracting 3 times with charcoal (10g/100ml ea) the difference was amazing.
 
 
 
 
    Aurelius
(Hive Addict)
03-03-03 22:29
No 413429
      Complete Writeup?     

Has a complete writeup of this procedure been produced?
 
 
 
 
    fierceness
(Hive Bee)
03-04-03 05:20
No 413555
      purity     

No.. neither Chromic nor I have gotten a suitably-pure end product for a writeup... and the whole nitrosamine question is rather disturbing.. it seems like most any acid will destroy nitrosamines, but there is a toxic-tasting substance (and smelling until some purification is done) in both of our runs..

It's bad enough we're poisoning ourselves with it ;)
 
 
 
 
    MinorThreat
(Stranger)
03-04-03 23:34
No 413826
      if you     

have a friend with a GC/MS setup available to him it might be worth while to see what the contaminant is, hell i could be something thats harmless and then it just tastes bad, and if you ran it and discovered which nitrosamines were present you could find a way of preventing the side reactions..
 
 
 
 
    pHarmacist
(Hive Addict)
03-04-03 23:48
No 413830
User Picture 
      Chromic     

Why don't you send a sample to a lab for analysis? There are those that make money on E-pill analysis, I'm sure they can run an analysis on your sample.

Accept No Imitations, There Can Only Bee One; www.the-hive.ws
 
 
 
 
    fierceness
(Hive Bee)
03-05-03 02:37
No 413943
      all the E-pill labs have strict rules on what...     

all the E-pill labs have strict rules on what they analyze.. they won't even analyze anything that isn't a pressed pill.. they require that one sends in like $100 when you even send in a capsule..

i dont think they will analyze a sample of GHB and an unknown contaminant.. if i'm wrong, please correct me.. i'm more than willing to send in a sample
 
 
 
 
    roger2003
(Newbee)
03-05-03 14:38
No 414046
      German Dissertation about industrial scale...     

German Dissertation about industrial scale production of
1,4 butandiole, g-butyrolactone and THF

http://www.ubka.uni-karlsruhe.de/vvv/2000/cheming/2/2.pdf
 
 
 
 
    MinorThreat
(Stranger)
03-05-03 18:08
No 414071
      umm     

we know this roger we are working on a synth that is far diffrent from those,as we are useing GABA as a starting agent and btw please translate what you post most bee's here do i beelive, blush
 
 
 
 
    Prdy2GO
(Hive Bee)
03-16-03 11:23
No 417558
      The GBL was great!     

Yes indeed the GBL was great only after tripple distilling the extracted product. Here are a few guide lines to get to GBL safe and cleen.
After the reaction is complete.
Distill off about half the volume at normal pressure. Use Methyleen Chloride to extract the GBL. Distill off the solvent and then get ready to vacumme distill after a 100 C or so I begin to reduce the pressure. Keep everything that will come over above 190C this is the first step of three. This product is then distilled and the fraction starting at 200C is kept the final distillation is at about 204 and this is clear clean GBL. Clean your glass between distillations do not use rubber or anything else to flavor your GBL Be safr and have fun. A good mix is to take 120Ml in a 32 oz bottle  and fill with water. 15ml in juice or half a glass of water is a heavy starting dose and 20 to 25 ml is like an OD MAN!!! dont drink Alchol with it or you will punish yourself...

WTF is that smell... It keeps following me.
 
 
 
 
    hCiLdOdUeDn
(Hive Addict)
03-26-03 01:07
No 421255
User Picture 
      Any updates chromic, anyone?     

About the purity of GBL from GABA. . .

Is it probable to obtain NaGHB or KGHB of reasonable & ingestiable purity from distillation of the crude tasting GBL and converting to NaGHB or KGHB by reflux with sodium bicarbonate or potassium bicarbonate?

Chemistry is hard to learn, but its worth it.
 
 
 
 
    fierceness
(Hive Bee)
03-26-03 05:33
No 421362
      so far, the crude tasting GBL that we've been...     

so far, the crude tasting GBL that we've been talking about leaves a strange taste on the NaGHB.. i'm still working on a reasonable way to purify it without having to do multiple distillations.. i have several ideas, i just haven't gotten around to testing them yet
 
 
 
 
    hCiLdOdUeDn
(Hive Addict)
03-27-03 04:34
No 421630
User Picture 
      SWIM needs to try this synth.     

SWIM needs to try this synth. He need's a good source for GABA first.

Chemistry is hard to learn, but its worth it.
 
 
 
 
    foxy2
(Distinctive Doe)
03-28-03 20:26
No 422075
User Picture 
      He need's a good source for GABA first. Google     

He need's a good source for GABA first.

Google
 
 
 
 
    aradan
(Stranger)
03-28-03 22:57
No 422097
      Not google, but froogle     

for GABA, try froogle (http://froogle.google.com)
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
03-29-03 10:54
No 422232
      Good site     

Excellent links are found with froogle to a variety of suppliers. My recommendations are quite simple:

1) avoid buying any GABA in a capsule/tablet
2) make sure the GABA dissolves in a minimum of water before running the rxn (ie 1g GABA/1-2g water) to make sure you've received the right stuff
3) avoid liking the GHB more than you like yourself
 
 
 
 
    aradan
(Stranger)
03-30-03 17:51
No 422529
      Gaba, no capsules, no tablets     

OK, this is my suggestion: (http://froogle.google.com/froogle?num=20&q=allintitle%3A+gaba+-caps+-cap+-capsules+-tabs+-tablets&btnG=Froogle+Search)
This pretty much excludes tablets and capsules
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
04-01-03 04:36
No 422946
      Along with that search...     

I found http://friendsoffreedom.org/article.php?sid=1242 It's a site trying to get among other things, GABA (a GHB precursor...) legalized for sale in Canada using a bee hive for their logo in the name of "Friends of Freedom".

Is this a Hive secret op? smile
 
 
 
 
    StraightEdge
(Hive Addict)
04-04-03 15:47
No 423882
      filtering gbl with activated charcoal?     

M3psych....when you say filtration with charcoal, what exactly do you mean? AF has tried mixing with a few capsules of the powdered form, but a coffee filter failed to remove the black color. Would a better lab filter do the trick? Brita filters seem to achieve the same goal but they are expensive. Are these larger granules used in Brita filters available in stores?

A lot of people seem to remain silent when the topic of activated charcoal is brought up. I'm guessing that's cause they think it is a dumb idea. Why is that?
 
 
 
 
    Rhodium
(Chief Bee)
04-04-03 17:07
No 423897
User Picture 
      Beehive Political Model     

StraightEdge: Charcoal does not work well in viscous solutions (and GBL is), that might be one of the reasons.

Chromic: Regarding the "Friends of Freedom" beehive:

The Plan (http://www.friendsoffreedom.org/ffinfo.htm)

• To develop a "Beehive Political Model" in each province, and territory of Canada, and each country in the world.

• Our concept is to create "Working Cells" in each jurisdiction that are capable of working as Freedom Advocates to ensure that the political, economic, and legal processes are supportive of our goals.

• United and organized we can change the political, economic, and legal processes to restrict the government's and corporations' arbitrary power to interfere with one of our most basic right - the right to clean air, clean water, healthy food, and the health care products, and treatments of our own choosing.

• We can also ensure that every taxpayer fully understands, and is empowered and equipped to assert their rights to defend themselves from exploitation and interference by the governments and corporations.

 
 
 
 
    gabd
(Hive Bee)
04-04-03 19:45
No 423912
      For a good source of activated charcoal     

Go to your local pet store in the fish section
Its used for filtering, and its pretty cheap!
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
04-06-03 22:21
No 424403
      Last reaction     

I've had to part from this synthesis for some time. The last reaction I saw a buddy perform was a 1.5mol batch.

Mixed 1.5mol GABA (154.7g), 750mL water & 1.5mol sodium nitrite (103.5g) in a 1L roundbottom flask with a 1.5" egg stir bar. The flask sat in an cold water bath of about 3L in volume. A pressure-equalized funnel was placed ontop, with a gas adapter stacked on top of that. The fumes were vented to the outside via rubber tubing (poisonous nitric oxide is produced).

0.75mol (75.1g) of sulfuric acid was measured out in a beaker. It was mixed with ice-cold water to a volume of ~150ml. About 20ml of diluted acid was added to the funnel and slowly dripped in (<1 drip / second) with stirring. No sooner than once an hour, another 20ml was added to the funnel and allowed to slowly drip. This took about 2 days as often more than one hour was waited and no attention paid to hurrying this reaction along. It can go faster, but don't add the acid in less time than 12 hours.

After the reaction stopped, and no more bubbling was seen (seen about 24hrs after the last addition of acid), 1.5mol (150.1g) of sulfuric acid was added. The flask was allowed to sit a further 6hrs or so, nothing was done to rush the reaction.

The reaction was extracted with 5x150ml methylene chloride. The DCM was distilled off. A yellow-brown liquid remained.

This was distilled in a flat-bottom flask at atmospheric pressure (insulate everything with glass wool) with a short column (vacuum distillation would have been ideal, but wasn't available). 92.3g (81.7ml, 1.07mol) of GBL was recovered around 198-202C. This was a yield of 72%. Certainly much higher than the first post in this thread.

Then 92.3g GBL (1.07mol) was mixed with 90.1g baking soda (1.07mol NaHCO3) and 370ml of water. This was simmered (i.e. a very light boil at 100C) for 30mins where NaGHB was formed. Then it was boiled down to a solid (without charring). Then it was rediluted with water.

The NaGHB still had an off-taste but was drinkable. I would recommend trying to filter with activated charcoal before serving but have never tried it.

As of right now, this is the superior method on the boards on how to make GHB via this method. Keep in mind this method has still not matured and is still experimental.

The main points are:

1) use 0.5L of water for 1mol GABA/NaNO2, add 0.5mol H2SO4 SLOWLY and in PORTIONS, then let sit for 24hrs+ after adding all the acid
2) acidify with H2SO4 and extract with an equal volume of DCM split into 5 portions
3) distill off DCM, then distill the GBL. (this is essential!)
4) convert to NaGHB, steam distill off the aqueous to remove impurities that don't react with baking soda, then redilute
5) consider filtering with activated charcoal
 
 
 
 
    M3Psych
(Newbee)
04-10-03 02:10
No 425298
      SWIM has had great success using the ...     

SWIM has had great success using the combination coffee filters which have a plastic shell (which wonderfully isn't eaten by GBL) and have a thin layer of AC in them. They are sold for removing chlorine and other bad tasting compounds from water so that your coffee doesn't taste like shit.

SWIM has found that this filtration improve the quality of the experience beyond anything he could have imagined. Every irritating aspect of GBL (except the acidosis) disappears and a crystal clear, euphoric and non-dizzy state is attained. Even the purest GBL isn't meant for human consumption so drinking without doing some sort of filtration is probably unwise. The heavy metal content, while probably not enough to cause acute injury certainly does have SOME effect, especially on the high. Arsenic, lead, mercury and other assorted nasties have no place in the human body, any amount is toxic.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
04-10-03 06:28
No 425338
      GBL     

I bet most GBL is purified by distillation before sale, I doubt that there are any heavy metals in it... however, the VOCs are worth worrying about.
 
 
 
 
    Daphuk_up
(Hive Bee)
04-12-03 04:06
No 425958
      Just mentioning...     

Just wanted to mention that SWID had some success with this reaction, substituting HCl for H2SO4.  A smaller initial batch was met with good success, and a bioassay of said material (1 gram) was excellent.  (Apparently the bioassayer had never before connsumed NaGHB, and was suprised and quite happy with the results. wink)  However, a second run on a 3x scale failed fairly miserably, for currently unknown reasons.  Reaction is to be attempted again, and SWID sees no useful purpose in relating his harrowing tale until he has mastered its telling.

Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
 
 
 
 
    Daphuk_up
(Hive Bee)
04-22-03 02:13
No 428530
      Oh.     

Mmm, SWID is a dipshit. shocked  He apparently treated the GBL with NaOH to make NaGHB, THEN tried to extract with isopropyl alcohol.  (The first successful run he used ethyl, second discrepency.)  Anyways, SWID believes this process is very viable using HCl instead of H2SO4.  SWID's bioassayer reported nothing in the way of a bitter or otherwise unpleasant taste in the NaGHB.  Salty was the only term used to describe it.  SWID would also like to mention that GABA doesn't taste that bad either, if that is indeed what SWID ended up extracting.

Anyways, something to think about.  (Something else to think about:  The Merck 11th states that NO2, that funny brown gas thats so often produced when acid is added a bit too quickly to the NaNO2 is a deadly poison, and one of the most insidious (is that emotion evoking descriptive term appropriate to a scientific publication?) gases known to man.  It can kill in the 200ppm range, or .02% by volume.  At the time little or no pain will be felt, and over the next 48 hours various severe respiratory problems lead to death.crazy)

Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
 
 
 
 
    hackertnv
(Stranger)
05-10-03 22:50
No 432540
      What to use as a DCM     

sup I was trying to make ghb from gaba and all I lack is a DCM. I know that you can use Methylene Chloride but I can not obtain it... Does anyone know a different thing I could use like toulne or xylene?  Maybe something that might be in a small chemistry class.
 
 
 
 
    ClearLight
(Hive Addict)
05-11-03 02:38
No 432556
      Since you already have everything setup...     

Take your addition funnel and load it w/ the gbl.  Create a molar EtOH + NaOH solution and heat to boiling. Slowly add your GBL to the mix, do this at about 2 drops a second.

  Monitor ph, when it hits about 7 you should have emptied your addition funnel ( if your ratios are right). Run the temp up to about 235 deg C and collect unreacted lactone ( if any).

   Pour hot NaGHB into pyrex dish that has been lightly sprayed w/ cooking oil ( or not if you want absolute purity but it REALLY sticks).

   Scrape up, vacuum pack (horribly hydroscopic), or toss in covered plastic container into fridge.

 Experimental:

  The following will fit nicely in a 500ml rb flask:

   40 ml gamma-butrylactone  (GBL)
   21 gms Sodium Hydroxide (NaOH)
  300 mls Ethanol (EtOH)

  Assemble a 500ml RB flask on the mantle, w/ a claisen adapter connected to an additional funnel on the side arm. Place a refluxing condenser connected to a cooling water flow on the straight arm of the adapter.

  Add 3-4 boiling stones to the RB Flask

  Mix the NaOH + EtOH in a 500 ml RB flask and bring to reflux

  Add the GBL via the addition funnel at the rate of 2-3 drops per second.

  After about 2/3's of the precursor material is added the contents of the flask will become milky white.

  Check the pH after GBL addition.  If the pH is at 7 your GBL was not pure or you mis-measured. If your pH is low, add via addition funnel in 10 ml portions additional GBL until the EtOH/NaOH/GHB solution is no longer basic.

  (Optional) If you wish to recover excess GBL, replace the reflux condenser w/ an adapter, thermometer and a liebig distillation condener. Discard everything before 215 deg. C.
  Collect the fraction between 218-232 deg. -> GBL

  Pour the flask now containing (while still hot and liquid) GHB into a pyrex baking dish and allow to cool. While still plastic and soft, scrap up into piles w/ spatula to avoid massive adhesion to surface. You can use a non stick pan and avoid the adhesion.

  Immediately vacuum pack the mass to avoid water uptake from atmosphere, or place in a plastic tupperware container and freeze.

   Dosage:  weigh 1.8 - 2.5 gms depending upon your tolerance and add to water.  Enjoy! smile

  The advantage of this method is that you have solid product at the end, you don't have to try and remember what a dose is, and no mold or slime forms as occasionally happens w/ liquid solutions.

Infinite Radiant Light - THKRA
 
 
 
 
    fierceness
(Hive Bee)
05-11-03 02:59
No 432563
      DCM = Methylene Chloride ether works.     

DCM = Methylene Chloride

ether works.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
05-11-03 14:42
No 432619
      solvents     

diethyl ether, ethyl acetate or methylene chloride will work. Benzene, toluene, xylene won't. Solvent extraction is the way to go... steam distillation will work somewhat.
 
 
 
 
    hackertnv
05-12-03 20:42
      So where do i get?
(Rated as: UTFSE!)
    
 
 
 
    fierceness
(Hive Bee)
05-12-03 21:02
No 432848
      UTFSE in the acquisitions forum...     

UTFSE in the acquisitions forum... diethyl ether can be obtained from starting fluid
 
 
 
 
    hackertnv
05-13-03 23:05
      ok ready....
(Rated as: no sources!)
    
 
 
 
    hackertnv
(Stranger)
05-18-03 23:37
No 434045
      All Ready (correct all mistakes in reply)     

OK this is how i plan to do it:
154.7g GABA mix with 750ml water & 103.5g sodium nitrite (how many ml would 103.5g be?)
place in 1L flask in 3l volume water.
75.1g sulfuric acid (how many ml? 40.1ml??) mixed with 150ml water
20ml diluted acid dripped 1 drop per second, into gaba mix.
hour later same thing, until no reaction of bubbling occurs.
then add 150.1g sulfuric acid(how many ml is that and is it the diluted acid? drop per sec again?).
then reaction extracted with 5x150ml ether (from starting fluid). then DCM distilled off with? boil it out? at what degree? or water?
insulate flask with glass wool heated at 198-202C to get gbl.
81.7ml of gbl mixed with 90.1g baking soda and 370ml of water.
boil at 100C for 30 min.
NaGHB Formed boil down to solid, then redilute with water.

all corrections just repost it please.
 
 
 
 
    Rhodium
(Chief Bee)
05-18-03 23:59
No 434049
User Picture 
      Densities     

103.5g sodium nitrite (how many ml would 103.5g be?)

Sodium nitrite is a solid, and it does thus not have a specified volume per weight unit - it simply depends on crystal size, and how loosely packed it is. Solid reagents always needs to be weighed out.

75.1g sulfuric acid (how many ml? 40.1ml??)

The density of 98% sulfuric acid is 1.84, so it would rather be 40.8mL (but maybe your acid maybe of a different concentration?).
 
 
 
 
    hackertnv
(Stranger)
05-20-03 18:40
No 434371
      thanks rhodium but....     

thanks for the sulfuric information..... but my sodium nitrite is in a bottle that we got from our chemistry class... so what do i do??? 103.5g to ml ?? how? or what???

D.P.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
05-20-03 19:44
No 434382
      Use a scale!     

USE A SCALE! Even a very cheap scale would be better than nothing. Don't attempt this experiment if you don't have the ability to:

1) weigh substances with at least 1g accuracy
2) distill high bp substances or vacuum distill (at the minimum steam distill)
3) direct the gases produced somewhere other than your living area

And if you still don't listen, then do not offer whatever you make to anyone but yourself... it will taste like near poison to drink.
 
 
 
 
    hackertnv
(Stranger)
05-21-03 01:26
No 434422
      k     

gottcha, i had it all ready, thats the reason i was wanting to know the exact thing in ml's b/c all i was gonna do is pour it in the flask and measure that way... w/the liquid shit anyway.. ill tell you how it turns out... i have a couple digital scales im using.
 
 
 
 
    Aurelius
(Hive Addict)
06-13-03 13:58
No 439754
      Final method?     

Hey Chromic, is this your final procedure for this method?
Post 432556 (ClearLight: "Since you already have everything setup...", Chemistry Discourse)

Are you still working to get a better product/higher yields or is this your finishing point?

Act quickly or not at all.
 
 
 
 
    ClearLight
(Hive Addict)
06-15-03 09:48
No 440118
      EDIT!     

The following line:
If the pH is at 7 your GBL was not pure or you mis-measured.

 Should read:
 If the pH is NOT at 7 your GBL was not pure or you mis-measured.

Infinite Radiant Light - THKRA
 
 
 
 
    hackertnv
(Stranger)
06-17-03 20:11
No 440601
      Diluted Sulfuric..     

Sup i was wondering when your going to add 75.1 g sulfuric acid in a beaker.... do u add ice cold water till it reaches 150ML or do you add 150ML water?
 
 
 
 
    Beaker_Is_Alive
(Stranger)
06-18-03 03:13
No 440644
      Thanks to all who put their time into this...     

Thanks to all who put their time into this project. We owe you one!

However, why wouldn't heating the GABA/NaNO2/H3O+ solution, with adequate ventilation, speed up the reaction to completion?

Thanks again.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
06-18-03 03:20
No 440646
      Hang tight     

Yes, this is my final procedure. Soon I will be able to reusme experimenting. Hang tight.

Add 150ml to the 75.1g sulfuric. Go slow, overheating can happen.
 
 
 
 
    Rhodium
(Chief Bee)
06-18-03 11:29
No 440786
User Picture 
      Always Add Acid to Water     

No! You cannot add water to concentrated sulfuric acid like that, it will boil and splatter! Better to add the sulfuric acid slowly to a weighed quantity of ice...
 
 
 
 
    whyohwhy
(Stranger)
06-18-03 15:13
No 440825
      Has anyone tried adding NaOH/Water to the...     

Has anyone tried adding NaOH/Water to the DCM/GBL? Does this work? I tried distilling the DCM/GBL but something went wrong. The DCM distilled over, everything left turned into a black solution. Anyone else had similar results?
 
 
 
 
    fierceness
(Hive Bee)
06-18-03 17:31
No 440852
      Yes.     

Yes... swif has tried this.. a nasty emulsion formed.. the emulsion cleared after a couple days, but i think the yield suffered greatly.

Do it as chromic outlined, and you will get product.
 
 
 
 
    Beaker_Is_Alive
(Stranger)
06-19-03 04:12
No 440942
      Okay, my friend tried to extract the GBL from...     

Okay, my friend tried to extract the GBL from the reaction mixture using ether obtained from Prestone starting fluid.

The pH of the reaction mixture was first tested and determined to be ~3; acidic enough.

An eq. volume of ether was poured over reaction mixture, covered, shaken, and allowed to sit for ten minutes. The ether over reaction fluid was shaken and allowed to seperate for ten minutes several times. No emulsion remained after the final shake/rest.

The reaction fluid was xfered, separated, and then returned to original pyrex flask via inverted 32oz plastic bottle with small hole in screw-top lid.

The remaining ether layer was quickly xfered to a seperate pyrex flask. The ether solu^n was, at this point, clear and blue. It had no color originally.

A dil NaOH solu^n was preparred and then used to titrate the ether solu^n. NaOH was added carefully and slowly with a flat piece of plywood (snuffer) and a fire extinguisher on hand.

A reaction is noted as H2 is produced. Addition of NaOH continues until bubbles no longer form.

The water/ether solution is then xfered to another 32oz with hole in screw-top and the bottom layer poured into a glass bowl via inverting the bottle. The ether solution is now clear and colorless, while the water layer, now in the bowl, is a clear, dirty-yellow color.

The water layer is pH's at 8, and baking soda is added until neutral/7.2.

The result?

NADA. The water layer is salty as hell, but upon sampling it is determined contains NO or very little NaGHB. However, it IS extremely salty, much more so than he thought it would have been, and does not taste at all like NaGHB. Two soda caps are taken. NADA.

My friend has no idea what went wrong. He thought for sure, after observing every step of the extraction and synthesis, that he had SOMETHING.

What could have been extracted in the ether that would have reacted with the NaOH when titrated? frown
 
 
 
 
    hackertnv
(Stranger)
06-26-03 00:29
No 442554
      at the end......     

ok at the end when u have your NaGHB and you boil it down to a solid do you add 370 ml of water to redilute? or more? its a 1.5 mol batch right?
 
 
 
 
    methyl_ethyl
(Hive Bee)
06-26-03 01:49
No 442570
      redilution     

ok at the end when u have your NaGHB and you boil it down to a solid do you add 370 ml of water to redilute? or more?

 If you alredy have NaGHB you just need to redilute it with whatever concentration of water that you want to make a dose. 
     I like 2.5grams NaGHB/dose, and I prefer to take that in a 30mL total liquid volume shot, just do the math.  I do this for ease of measurement.  So when I want a 2.5g dose of NaGHB I pour myself an easy to measure shot, or draw up  30 mL in a syringe, or a fucking pipette if your real anal.
     Well I do not really do that I just take swigs from the bottle, but until you become best friends with this stuff, measure it out with accuracy, and always measure if it is for someone else....  You will then know the true meaning of Unipolar Mania laugh

     Unipolar Mania, It's good for life...laugh
 
 
 
 
    whyohwhy
(Stranger)
06-27-03 19:56
No 442969
      After following this post and with some help...     

After following this post and with some help from a few others, a newbee like myself was able to synth gbl. I just wanted to post my thanks ... chromic & fiercness you guys are awesome.
 
 
 
 
    hackertnv
(Stranger)
07-02-03 14:42
No 443992
      liquid nitrite     

to make sure i don't mess up im asking 1 more question.... if i need 103.5g sodium nitrite.. and if my sodium nitrite is in a liquid form.... then should i just put the flask on the scale and pour in till i get 103.5g adding weight for the flask or should i just add 100ml of it?
 
 
 
 
    Rhodium
(Chief Bee)
07-02-03 16:02
No 444008
User Picture 
      Sodium nitrite is not a liquid, it's a solid.     

Sodium nitrite is not a liquid, it's a solid. What you have must be a solution, so you must either remove the water or find out the actual sodium nitrite concentration of that solution and calculate how much you should use.
 
 
 
 
    methyl_ethyl
(Hive Bee)
07-02-03 20:10
No 444066
      solution     

All of the solutions I have seen are usually 40% sodium nitrite and water.  How do you know what you have is sodium nitrite, is the label still affixed?, if it is, it should say rite on the label the %solution you have.  And if you can not figure out how much to add with the amount of solution you have, you may want to quit the reaction and pick up a few chem books. 
     Also make sure your label does not read Sodium nitrite oxidizing salt solution.  This can not be used as it contains sodium nitrate 20%, and sodium carbonate 2% also.  I am not a chemist but I would beelieve that this would interfere with the reaction.  

or should i just add 100ml of it?

I have no idea where you pulled this figure from.

     Unipolar Mania, It's good for life...laugh
 
 
 
 
    hackertnv
(Stranger)
07-04-03 01:05
No 444345
      Nitrite Solution     

k so if i have sodium nitrite solution.... which is a liquid what should i do?? if i have to ill order some sodium nitrite, but i already have the solution here... it doesn't say the % of sodium nitrite in it, but it does have the label. The chemistry safty guide is 20010, thats the only thing that it really said other than the name, besides the warnings.
 
 
 
 
    catfish
(Hive Bee)
07-05-03 08:39
No 444655
      substitute solvents     

Hi all-
SWIM has access to several solvents, but the dihaloalkanes are not among them.
In theory, how would tetrachloroethylene compare to DCM, et al. How about 1,1,1-trichloroethane? And there is one industrial solvent that SWIM cannot recall the proper name for- "Carbosol". Would methyl carbitol bee appropriate? Monochlorotoluene?
I realize this is somewhat broad question, but I believe that the broader the application of solvent utility, the longer this synth will be OTC and a viable alternative to street (read "dirty") drugs.
All replies welcome, but please do not ask me where to get these solvents, since I am not SWIM.
-catfish

all information related for educational purposes only!
 
 
 
 
    catfish
(Hive Bee)
07-05-03 08:53
No 444658
      GABA.HCl?     

Hi all-
SWIM had one last question for the morning...is the proper form of GABA is the hydrochloride?
If so, does this mean that the mole of HCl must bee accounted for (i.e. subtracted from) when figuring molar ratios, or does the procedure account for the fact that most GABA comes as the hydrochloride?
CRC Handbook: butyric acid, 4-amino or piperidinic acid crystals- prisms or needles from dil alcohol, leaves from metanol; mp 203'C (decomposes); soluble in water.
Thx in advance.

all information related for educational purposes only!
 
 
 
 
    gabd
(Hive Bee)
07-05-03 16:56
No 444709
      I dont think so     

It's straight GABA, Mw of 103.120, C4H9NO2
No HCL
At least from chem suppliers, its advertised and sold that way.
 
 
 
 
    hackertnv
07-05-03 23:26
      Nitrite Solution
(Rated as: Already asked 4 posts up)
    
 
 
 
    fierceness
(Hive Bee)
07-06-03 01:11
No 444797
      you need to know the percent NaNO2 in the...     

you need to know the percent NaNO2 in the solution.. guessing at that point may prove bad for your health.. NOx gasses are bad for your health
 
 
 
 
    hCiLdOdUeDn
(Hive Addict)
07-06-03 21:06
No 444981
User Picture 
      Rhodium....     

How come this synth hasent come to the pages at your website?

Chromic...Have you made a finished writeup on this synth yet?
 
 
 
 
    Rhodium
(Chief Bee)
07-07-03 00:47
No 445036
User Picture 
      Recursive answer     

hCiLdOdUeDn: The answer to the first question is "Because the answer to the second question is no". wink
 
 
 
 
    hCiLdOdUeDn
(Hive Addict)
07-07-03 04:17
No 445094
User Picture 
      Chromic!!     

Please write a writeup!!! We are all counting on you!smilesmile
 
 
 
 
    hackertnv
07-08-03 20:51
      Would This Work?
(Rated as: no sources!)
    
 
 
 
    Tdurden969
(Hive Bee)
07-08-03 22:56
No 445695
      What the fuck     

See the front page

"No trading or discussion of commercial suppliers. "

What part of NO SOURCES don't you understand.
You're obviously not a hacker cause that usually requires some common sense mad
 
 
 
 
    methyl_ethyl
(Hive Bee)
07-08-03 23:07
No 445697
      yes     

That would be it, and that would also be posting a source.  But it is not up to me to tell you that....

     Please do not run this reaction without proper ventilation.  Seriously,   The gasses that are evolved from this reaction are extremely Toxic.  This may be the easiest way to get ghb from otc chems, but it is probably the most dangerous if you do not have proper ventilation, I know this has been said 1,000 times but, please do not attempt this in your house.  

     I fear for your life.. frown

     Unipolar Mania, It's good for life... laugh
 
 
 
 
    JonnyDanger
(Stranger)
07-09-03 00:03
No 445708
User Picture 
      Please delete your post Hack     

NO SOURCES... This rule is there for a reason. Its to protect businesses. By posting that you put that company at risk (or at risk of being watched if nothing else). Please delete it immediatly... moderators? cool
 
 
 
 
    yobkcis
(Stranger)
07-10-03 18:12
No 446242
      Please give us a writeup -- or a SO FAR...     

I have read through most of the posts on this topic, and I must say i am really unsure of how to get to the finished product. (I am a newbie and i failed science in jr. high frown)...  can anyone give us a short and sweet but accurate version of exactly how to get GBL using this method, including all the things learned since the initial post was made?

Thanks, and pardon me if i'm out of line asking for this.
 
 
 
 
    JonnyDanger
(Stranger)
07-10-03 20:36
No 446256
User Picture 
      GABA --> GBL --> GHB In layman's terms     

I'll try to explain the method in layman's terms as I understand it... The highest lvl of chemistry education I have is highschool but I've read all the posts and did a lot of research on the internet as well... so here goes smile:
(Oh, and if get anything wrong, someone pls let me know and I'll edit the post to reflect that)

Ingredients needed (which can all be purchased online on various websites): 154.7g pure GABA, 103.5g Sodium Nitrite, 225.2g Sulfuric acid, 750ml DCM, 90.1g baking soda (or Sodium Hydroxide, not sure on exact amount though) and Distilled water.

Equipment needed (All of which can also be purchased online): high temp thermometer (at least 210c max temp), 1 1L capacity, flat bottom Erlenmeyer flask, 1 distilling set up, 1, 1L capacity seperatory funnel (for the separation process and the acid dropping process), 1 Bunsen burner or similar heating apparatus (a propane torch maybe?) one large bowl (at least 3L capacity), PH testing strips, and safety equipment (i.e. safety goggles, gloves, apron).

PROCESS:

1: In the 1L Erlenmeyer flask, mix the GABA, Sodium Nitrite, and 750ml water.

2: Set that mixture (inside of the Erlenmeyer flask) in the large bowl with water and ice and allow to cool.

3: In the separatory funnel, add about 120 ml ICE COLD water. Then SLOWLY add 75.1g sulfuric acid.

4: Rig the separatory funnel so that its above the Erlenmeyer flask and may drip into it. Allow the sulfuric acid mixture to slowly drop into the GABA/Sodium Nitrite mixture (NO MORE THAN ONE DRIP/SECOND and no more than 20ml/hour). NOTE: This process should be done outside or with very adequate ventilation as a VERY poisonous gas is produced by the reaction.

5. Let sit for 24 hours or until no more bubbling is seen.

6. Add another 150.1g of sulfuric acid to the mixture. (Not sure one the addition time or if water should be mixed with the sulfuric acid first... some help here? wink) Let sit for 6 hrs.

7. Clean the separatory funnel.

8. In the separatory funnel, mix 150ml DCM and the GABA/sulfur/sodium mixture and shake well.  Allow to sit until separation can be seen (2 layers of liquid). Remove the DCM portion and SAVEwhich will be the bottom portion. Discard what is remaining in the sep funnel. Take the DCM portion and repeat step 8 until no DCM remains (5 times). (if any part of this step is wrong or could be explained more clearly, let me know and I will modify it)

9. Combine the multiple DCM separations.

10. Boil off the DCM till only the GBL remains (which should be yellow/brown liquid.

11. Distill the GBL in your distilling apparatus at 198-202C. (If someone wants to make a full write up of the distilling process I will add it)

12. Mix 90.1g baking soda and 370ml distilled water.

13. Simmer GBL and baking soda mixture at 100C for 30 min to balance the PH by forming NaGHB. (I prefer to use NaOH for this step)

14. Redilute with water to desired potency.

15. (optional) (Thanks to hCiLdOdUeDn for providing the following smile) You must boil the impure, nitrosamine contaiminated, NaGHB in solution with a few grams of activated charcoal for a few mintues, with good stirring (magnetic stirbar reccomended). The activated charcoal will absorb the impurities.

For the cleanup of the impure GHB, I reccomend:

1) Boil the NaGHB with activated charcoal for a few minutes
2) Filter this through a 5mm thick layer of celite.
3) Boil off the water from the filtrate and weight out the NaGHB
6) Add 190mL of water per 20g of NaGHB
7) Acidify with sulfuric acid to convert NaGHB to GBL
8) Steam distill (or simply distill) the entire mixture. All the GBL will come over with the water.

This dose is: 15mL of the distillate will contain 1g of GBL.
-----------------------------------------------------------

Once again, pls let me know of any mistakes/misleading statements as I have just woken up so I'm sure there will be smile
 
 
 
 
    Lilienthal
(Moderator)
07-10-03 20:43
No 446257
User Picture 
      NEVER add water to concentrated sulfuric acid!     

NEVER add water to concentrated sulfuric acid! crazy Always add sulfuric acid slowly with stirring into water! Please could you correct your post?

DCM will almost always be the bottom layer due to its high density.
 
 
 
 
    JonnyDanger
(Stranger)
07-10-03 21:19
No 446262
User Picture 
      Done, Thank you :-)     

Done, Thank you smile
 
 
 
 
    yobkcis
(Stranger)
07-10-03 21:38
No 446269
      Thanks     

Thanks very much for the summary.
 
 
 
 
    hCiLdOdUeDn
(Hive Addict)
07-10-03 23:22
No 446283
User Picture 
      Proper use of activated charcoal
(Rated as: excellent)
    

You dont filter through activated charcoal. You must boil the impure, nitrosamine contaiminated, NaGHB in solution with a few grams of activated charcoal for a few mintues, with good stirring (magnetic stirbar reccomended). The activated charcoal will absorb the impurities. You dont filter throught activated charcoal...that would be absolutley pointless.

For the cleanup of the impure GHB, I reccomend:

1) Distill the GBL
2) Convert to NaGHB or KGHB
3) Boil the NaGHB with activated charcoal for a few minutes
4) Filter this through a 5mm thick layer of celite.
5) Boil off the water from the filtrate and weight out the NaGHB
6) Add 190mL of water per 20g of NaGHB
7) Acidify with sulfuric acid to convert NaGHB to GBL
8) Steam distill (or simply distill) the entire mixture. All the GBL will come over with the water.

This dose is: 15mL of the distillate will contain 1g of GBL.

Enjoy!!
 
 
 
 
    JonnyDanger
(Stranger)
07-11-03 00:18
No 446286
User Picture 
      Re: Proper use of activated charcoal     

Is the step where the NaGHB is converted back to GBL and redistilled necessary? Or is that simply if you want GBL instead of NaGHB?
 
 
 
 
    JonnyDanger
(Stranger)
07-11-03 00:40
No 446289
User Picture 
      Oh! Oh! What about...?     

What about adding the activated charcoal, boiling and stirring, before step 11 in my write up? Would that work? I know it probably wouldn't work AS well... but would at least remove more imputities than just distilling alone...
 
 
 
 
    OcoteaCymbarum
(Stranger)
07-12-03 18:42
No 446659
      Uses for gbl
(Rated as: good read)
    

The main use of butyrolactone is as an intermediate in the synthesis of N-methylpyrrolidone (NMP) [23], pyrrolidone [24], herbicides (e.g., MCPB = g-2-methyl-4-chlorophenoxybutyric acid) [25], growth regulators (e.g., a-(4-methylbenzylidene)-g-butyrolactone [5418-24-6] [26]), a-acetobutyrolactone (a vitamin B1 intermediate) [27], and the rubber additive thiodibutyric acid [28]. Butyrolactone is used as a solvent for polymers [29], [30] and as a polymerization catalyst [31]; in hairwave compositions [32] and sun lotions [33]; and in pharmaceuticals [34]. It is also used in printing inks, e.g., for ink-jet printing [35], as an extractant in the petroleum industry [36], as a stabilizer for chlorohydrocarbons [37] and phosphorus-based pesticides [38], and as a nematocide [39]. More recent applications are in the electronics field as a cosolvent for capacitor electrolytes [40] and as a cosolvent for photoresists [41].

[23]  I.G. Farbenind., DE-AS 694043, 1938 (C. Schuster, A. Seib).
[24]  BASF, GB 1312463, 1973 (W. Himmele, E. Hofmann, H. Hoffmann).
[25]  Chem. Age London 71 (1954) 1239.
[26]  S. Huneck, K. Schreiber, DD 112884, 1975.
[27]  W. Reppe, Justus Liebigs Ann. Chem. 596 (1955) 163 – 164.
[28]  BASF, DE 917247, 1952 (W. Reppe, H. Friedrich).
[29]  Phillips Petroleum, US 2 958 677, 1960 (R. F. Kleinschmidt).
[30]  DuPont, US 3 000 844, 1961 (I. M. Bro).
[31]  Mitsubishi Petrochemical, JP 8129881, 1981.
[32]  Shiseido, DE-OS 2421248, 1974 (K. Ono, K. Torii, T. Ozawa).
[33]  BASF, EP-A 44970, 1982 (F. Thoemel, W. Hoffmann, D. Degner).
[34]  W. Klunk, A. C. McKeon, Science 217 (1982) 1040 – 1042. W. Klunk, D. F. Covey, Mol. Pharmacol. 22  (1982) 431 – 437. Grissmann Chemicals, GB 2028653, 1980 (E. Diethalm).
[35]  Whittaker Corp., DE-OS 2936241, 1980 (I. R. Mansukhani).
[36]  Esso Research, US 3013962, 1958 (Ch. N. Kimberlin Jr., W. J. Mattox). P. Alessi, I. Kikic, Int. Congr. Scand. Chem. Eng. Proc. 1980, 366 – 373.
[37]  DuPont, US 2958712, 1958 (F. W. Starks).
[38]  Dow Chemical, JP-Kokai 7986618, 1979.
[39]  GAF, US 3086907, 1958 (F. A. Hessel).
[40]  Nippon Chemicon Corp., EP 543 311, 1991 (Y. Yokoyama, T. Tsuji, M. Ue, T. Sato).
[41]  Samsung Electronics Corp., DE 19 720 413, 1997 (S. Chon et al.).

Taken from Ullmann's encyclopedia of industrial chemistry
 
 
 
 
    Aurelius
(Active Asperger Archivist)
07-12-03 19:02
No 446665
      Thanks!     

Makes a good addition to my digest!

Act quickly or not at all.
 
 
 
 
    hackertnv
(Stranger)
07-29-03 17:01
No 450573
      Extracting with Ether..     

When you have to extract gaba/sulfuric mix with DCM.. what do you actually have to do?? just add 150ml then heat? and do the same process over and over, until a yellow-brown liquid remains?
 
 
 
 
    yobkcis
(Stranger)
07-29-03 19:27
No 450591
User Picture 
      Electronic Grade GBL for ingestion     

Would Electronic Grade GBL (99.9% pure) --or so they state-- be suitable and safe for making NaGHB and to ingest? I don't plan on trying any GBL straight up.  Should i try to filter this by one of the methods above before making NaGHB?  Any comments/suggestions would be helpful.  Thanks.
 
 
 
 
    fierceness
(Hive Addict)
07-29-03 20:58
No 450598
      yes.. 99.9% GBL for NaGHB is fine.     

yes.. 99.9% GBL for NaGHB is fine.
 
 
 
 
    hackertnv
(Stranger)
07-31-03 17:49
No 450924
      Need Info Quick.!     

I need some information quick on what you actually have to do with the DCM.  I'm about to pour in the pure sulfuric.  What do i do with 5x150ml Ether.?
 
 
 
 
    methyl_ethyl
(Hive Bee)
08-01-03 02:20
No 450973
User Picture 
      Oh Boy     

I need some information quick on what you actually have to do with the DCM.  I'm about to pour in the pure sulfuric.  What do i do with 5x150ml Ether.?

     I was in the middle of replying to this post when I realized you will probably not be alive to read this.  So I end abruptly.

     Good Luck,

     methyl_ethyl

     Unipolar Mania, It's good for life... laugh
 
 
 
 
    hackertnv
(Stranger)
08-02-03 04:38
No 451174
      Gaba Run     

Well everything came out ok. except the PH was around 9.57. I didn't test it untill after it was already crystalized :( so that was a mistake. Oh and sorry methyl, but I didn't die from it, it was very weak tho.. i took 2.8g & it just increased my buzz i already had going, so i took 1.2 more and still did the same thing just made it last longer.  Any tips on what I might of did wrong? DCM to weak? I used diethyl Ether.
 
 
 
 
    StraightEdge
(Hive Addict)
08-06-03 03:33
No 451988
      questions about purification w/ activated charcoal     

hCiLdOdUeDn- Did you have a particular reason for converting to GHB before purifying?

Also, does this purification get out the bad taste that was reported in the first few tries of this method?
 
 
 
 
    JonnyDanger
(Newbee)
08-07-03 23:59
No 452362
User Picture 
      GBL doesnt filter well with activated ...     

GBL doesnt filter well with activated charcoal. Thats why you convert to GHB first

One sec, now I have to shit again...
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
08-08-03 04:35
No 452401
      Success?     

Does anyone know if the activated charcoal removes the aweful fishy/bitter taste of the end GHB? I sometimes wonder if it was just due to problems with my sulfuric acid (drain cleaner). I wish I could experiment with this, but for me to bring drugs into my vicinity would likely spell an end for my life as I know it.
 
 
 
 
    fierceness
(Hive Addict)
08-08-03 05:31
No 452414
      h2so4     

i was also using drain cleaner as my H2SO4 source... i got much better results using HCl.. however, i am also unable to do anything with this synth or any synth for awhile..  someone carry on the torch :)
 
 
 
 
    jammin
(Stranger)
08-11-03 16:18
No 452997
      HCl replacement of H2SO4     

I've got some 30% HCl i plan to use instead of the H2SO4 in the reaction. But what will be the right amount of HCl to add?

-jAmmin
 
 
 
 
    StraightEdge
(Hive Addict)
08-12-03 05:57
No 453082
      i haven't done this, but I'll try to help     

If I understand correctly, acid was added in both steps 3 and 6 (I am referencing Post 446256 (JonnyDanger: "GABA --> GBL --> GHB In layman's terms", Chemistry Discourse)). In step 3 the amount added was half the amount of GABA (in moles, not grams). In step 6 the amount was equal to the amount of GABA. For example, if you were using 1 mole of GABA, you would add .5 mole of sulfuric acid in step 3, and 1 mole in step 6.

With HCl you will need to add twice as many moles because it gives half the amount of hydrogens, per molecule. So for every mole of GABA you are using, you need one mole HCl for step 3, and two moles for step 6.

This information may be underneath your level of expertise, but I do not know what that is so I may have provided more than was necessary.
 
 
 
 
    Rhodium
(Chief Bee)
08-12-03 15:54
No 453117
User Picture 
      Huh?     

This sounds strange: Post 452362 (JonnyDanger: "GBL doesnt filter well with activated ...", Chemistry Discourse)

JohnnyDanger: How do you mean when you say it doesn't "filter well"? It sure must pass through the carbon? Or does it bind that well even if eluting with a non-polar solvent afterwards?

Edit: I might need to clarify myself here (after a suggestion in PM). In Post 423897 (Rhodium: "Beehive Political Model", Chemistry Discourse), my point was that I believe that undiluted GBL will be inefficiently purified by stirring with charcoal due to its oily and slightly viscous nature*, but that does not prevent any charcoal suspended in GBL from being filterable. Maybe Johnny's usage of the word "filter" was wrong and should read "purify" instead?

* It will work a lot better if you dilute the GBL to 20-25% or so in a suitable (low-boiling, non-polar) solvent though, but converting it to GHB first might be even better to achieve as high purity as possible. As GHB is an acid, maybe a bona fide acid/base extraction is the best purification method (but don't skip the activated carbon nor the distillation of the GBL).
 
 
 
 
    StraightEdge
(Hive Addict)
08-18-03 01:10
No 454225
      FYI - activated charcoal     

For anyone who is interested, filtering NaGHB in activated carbon reduces yield by about 10%. Maybe less if you are careful. So it seems like an acceptable decrease in yield, considering the (possible) increase in purity.

I will try to write a procedure for a bona fide acid/base extraction (whatever that is) of GHB, in the hope that it will jump-start interest in this thread again. We are very close to getting pure GBL by this method, it is only a matter of time. I wish I could do more but at the moment the most advanced equipment I can safely have is a glass saucepan and a stove element.
 
 
 
 
    StraightEdge
(Hive Addict)
08-19-03 05:41
No 454473
      never mind     

I read over some posts on acid base extractions for a little while but couldn't figure out how to apply the procedure to NaGHB. Post 286519 (MaDMAx: "LOOK! Recrystallization and A/B general info", Newbee Forum) is targeted towards drugs that have amine groups. I tried to follow it anyway, but it seems like it revolves around the extraction of the freebase rather than the acid, which it the opposite of what you would want for GHB.

But how would you get at the acid in the first place? Adding HCl to aqueous NaGHB would convert back to GBL, and adding NaOH would do nothing except make the solution more basic. 

GBL in water forms a 50/50 mixture of GHB acid and GBL, correct? Might this be of any use, i.e. could just the GHB acid be extracted from this mixture?

Is this post of any relevance to our problem?
Post 65036 (foxy2: "Re: GHB-->GBL", Chemistry Discourse)
 
 
 
 
    Rhodium
(Chief Bee)
08-19-03 12:13
No 454516
User Picture 
      A/B of GHB/GBL     

Exactly, you are supposeed to do it in the opposite way compared to an acid/base wash of an amine.

Compare the behaviour of the different substances at different pH's, and the solubility in water and non-polar (NP) solvents:

  Standard Amine GHB/GBL
When basifying to pH > 11 Water insoluble, NP soluble Water soluble, NP insoluble
When acidifying to pH < 3 Water soluble, NP insoluble Water soluble (good), NP soluble (better)


The difference only being that an acidified GHB/GBL solution is both soluble in water and in NP solvents, as opposed to a basified amine, which is essentially only NP soluble in most cases. To make the GHB/GBL migrate to the NP layer in an acid solution, we need to force it there, which is effected by adding brine (concentrated NaCl solution) to the aqueous layer to push the GHB/GBL out of it, as well as extracting several times with a rather large amount of a powerful NP solvent (DCM or chloroform). You have to determine experimentally how many and how big extractions are necessary to extract it all. When all of the product mixture has been extracted to the NP layer, the GHB acid will almost exclusively have been transformed into GBL.

Edit: Read more about "solvation power" here: Post 453146 (Rhodium: "Factors influencing choice of solvent", Newbee Forum)
 
 
 
 
    StraightEdge
(Hive Addict)
08-20-03 03:10
No 454612
      thanks for your help     

So an acid/base extraction of GHB/GBL would involve:

1) Extract acidified GHB/GBL solution to DCM (each time adding brine to force all GHB/GBL out), several times
2) Discard water layer
3) Extract GHB/GBL from DCM into an NaOH solution
6) Discard DCM layer
7) Repeat as necessary

Is this correct? There is one thing about it that doesn't seem right. When doing just the simple GBL+NaOH reaction I have noticed that the GBL (90% GBL solution to be specific) will sit on top of the NaOH solution in a layer, until it is heated to 100C. i.e. it does not seem to be soluble in the NaOH. Would this be a problem in this instance? Or at a certain point, say 50% GBL solution, does it become miscible with NaOH solution?  

In Post 49492 (Cheapskate: "Re: THF -> GHB Research", Chemistry Discourse) and Post 396342 (fierceness: "Re: I'd really recommend trying to reduce the...", Chemistry Discourse) recrystallization was suggested as a way to purify NaGHB. Maybe that is worth a try?

I would like to write a procedure that combines the four methods (distillation, acid/base extraction, activated charcoal, recrystallization) and is more accessible to the newbee. That way there will be fewer questions, and hopefully more will be encouraged to try it, report back their results, etc. But I just wanted to confirm I had the basics right before starting on that.

Or maybe the problem is not a lack of ideas but instead a lack of people to try them out. There is nothing I can do about that for the time being, but I should be moving in a month to a place where I will feel more comfortable having a setup. At that point I will be able to try some of these techniques and report my results.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
08-20-03 20:33
No 454736
      A/B problems!     

Did anyone notice that GBL and NaOH was exothermic and didn't take place until there was a higher temperature? I wouldn't feel comfortable with such an acid base extraction in DCM? Perhaps I worry too much.

Washing the NaGHB with DCM might be a good idea to remove organics that don't react with the base...
 
 
 
 
    CainTwister
(Newbee)
08-22-03 14:11
No 455036
      Duh     

After half a dozen synths, I prefer this variation;

Add your dry GABA in tenths to the HCl(aq) + NaNO2(aq) + H2O(l) mixture after first chilling the acid/salt solution in the freezer until slushy. Between additions, attach a condensor and stir magnetically over low heat for an hour or so under a hood; cork the condensor between additions to keep smog from escaping while your flask + contents are again chilled.

Yield is greatly improved. I actually ran five open air, two-dayers' before trying this blush
 
 
 
 
    StraightEdge
(Hive Addict)
08-23-03 06:39
No 455155
      is there still a bad taste?     

CainTwister - Have you found that any of the purification methods discussed in this post remove the bad taste from the final product?
 
 
 
 
    CainTwister
(Newbee)
08-24-03 16:27
No 455409
      Re: CainTwister - Have you found that any of...     


CainTwister - Have you found that any of the purification methods discussed in this post remove the bad taste from the final product?




Well, seeing as how I'm actually making all this up (I'm a writer of fiction and all of my posts are fictional), I can only guess about the taste.

Good works of fiction are almost always those the reader is drawn into when read, the reader responding as if what is written was, in fact, real.

However, try and forget that I am making it all up as I answer your question below.


Fractional distillation is the only way I have been able to improve the flavor, which can only be described as "piss-like." I firmly believe that urea is a byproduct of the reaction, or something similar. Yield is affected, though.

 
 
 
 
    StraightEdge
(Hive Addict)
08-25-03 00:30
No 455470
      to confirm     

So in your fictional dream, you tried acid/base extraction, activated charcoal, recrystallization, and washing the NaGHB with DCM, and found them to offer no improvement over the final product that could be had with just repeated fractional distillations. Correct?

Chromic, for me NaOH + GBL does not seem to take place until the temperature is pretty high, much higher than the boiling point of DCM. That is why I was wondering whether more water in the reaction vessel would lower the amount of heat needed, by allowing the two reactants to mix better. But looking at it now, that idea doesn't seem to make much sense.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
08-25-03 02:18
No 455478
      Maybe just a DCM wash?     

My preference for the A/B extraction would be to: take the post-reaction mixture and acidify as usual, extract with dcm as usual, distill the DCM off as usual, add aqueous base, wash with DCM, acidify, extract with DCM, then fractionally distill... then enjoy the GBL.

Alternatively skipping an A/B, one could do it as posted originally, but wash the NaGHB product with some DCM at the end. (then boiling down the volume of the NaGHB to remove all traces of DCM from the aqueous before ingesting) Perhaps the DCM would remove the stinky organics.
 
 
 
 
    CainTwister
(Newbee)
08-25-03 05:52
No 455507
      Re: So in your fictional dream, you tried...     


So in your fictional dream, you tried acid/base extraction, activated charcoal, recrystallization, and washing the NaGHB with DCM, and found them to offer no improvement over the final product that could be had with just repeated fractional distillations. Correct?




Actually, I haven't tried all that yet. blush

 
 
 
 
    StraightEdge
(Hive Addict)
08-25-03 06:53
No 455518
      I wish I could actually try some of these things     

But wouldn't distilling off the DCM in the middle of the acid-base extraction defeat the purpose? I thought the goal of the procedure was to have the impurities stay in the DCM. But if it is distilled, they will stay in the GHB/GBL mixture.

Did you ever get around to doing TLC on your product? Not that I think it would give a lot of useful info, I'm just curious.

As far as using HCl instead of H2SO4, Post 428530 (Daphuk_up: "Oh.", Chemistry Discourse) and Post 452414 (fierceness: "h2so4", Chemistry Discourse) seem to indicate positive results.

I am still not able to do any chemistry right now, but hopefully that will change in the near future. I guess what I will try is doing all of the purification methods (a/b, charcoal, recryst., DCM wash, frac. distill) at once, and seeing what the final result tastes like. If it is bad, I will probably just give up. If not, I will try again, each time doing one less purification until I find out which technique is working.
 
 
 
 
    shockwave
(Stranger)
08-25-03 15:46
No 455570
      A little vague     

I have seen some positive reactions to the use of HCI over H2SO4. It seems vague in certain details (any change in the method, a consistent amount, and a consistent concentration). HCI was also substituted in the early part of the thread but it seems that it has been forgotten. I would like to look into the HCI concept to see if there is any actual progress. Otherwise, does anyone know what's the most suitable drain cleaner out there? frown
 
 
 
 
    StraightEdge
(Hive Addict)
08-25-03 19:20
No 455610
      Reactant: 4-amino-butyric acid Products: ...     

Reactant: 4-amino-butyric acid
Products: dihydro-furan-2-one (70%), 4-hydroxy-butyric acid (30%)
Reagents: NaNO2, HCl
Solvent: H2O
Time: 24 hour(s)
Other Conditions: Ambient temperature
Reference: Bull.Soc.Chim.Fr.; 1; 88-94 (1989)

The reference says to uses HCl, so perhaps it would be best to stick with that if possible. That is, unless it was just chosen arbitrarily. But I don't have enough chemistry knowledge to know whether it was or not.

These posts are what led to the switch to H2SO4: Post 386749 (Chromic: "Steam distilling", Chemistry Discourse)
Post 387717 (Chromic: "I made another mistake", Chemistry Discourse)

The reason is not clear, but I am guessing it was because of improved yields or purity.

Or even if switching back to HCl is a bad idea for some reason, why not use better quality H2SO4 from a chem supply? It seems like it would be a good idea to start out with the purest reagents possible, especially given that the average dose of GHB/GBL is 10-50 times higher (by weight) than that of most drugs.

If anyone does try reverting to the HCl method, Post 375615 (El_Zorro: "So even if the freebase, is soluble in water, I ...", Chemistry Discourse) warns that problems may occur unless extra HCl is used. To find out whether or not this is the case, you could try adding acid until the pH is 4-5 like the reference (Post 375754 (Chromic: "Yields", Chemistry Discourse)) says. Record how much you added (in moles) and compare it to the amount specified in the procedure that uses H2SO4.
 
 
 
 
    fierceness
(Hive Addict)
08-26-03 23:25
No 455852
      A/B'ing the final product with no distillation     

A/B'ing the final product with no distillation yielded a nasty emulsion for swif.  It cleared up within a week, but it destroyed the yield.  I don't recall the exact numbers, but they weren't good.  Don't use drain cleaner for the H2SO4 if you can avoid it.  There was something in the one that swif used to hinder the reaction.
 
 
 
 
    shockwave
(Stranger)
08-27-03 02:41
No 455889
      One small step... You know the rest     

The creators of this thread have accomplished a lot in their concept. The hypothetical concept can go further though. It must be more abstract to compensate for the current political structures. I feel it may be posssible to use a quality H2SO4 in this abstract but I also feel that other parts are coming under more scrutiny.

Basically, I would like to take the concept further as far as quality (such as H2SO4 situations) and improved yield (such as HCI situations). I still will not come even close to the contributors and creators of this thread.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
10-01-03 22:15
No 462146
      Final word on activated charcoal
(Rated as: good read)
    

Okay, HCl was tried all the way thru instead of sulfuric acid. The results are the same. The distilled product still didn't taste right. It was not the acid that was at fault. In fact, I still recommend H2SO4 over HCl.. especially for acidifying the aqueous before extracting with DCM. I wouldn't really know much about doing this though, as it wasn't me who did these experiments.

By the way, do NOT try to scale back the amount of DCM used. For a 1 mol run, you really do need to use a total of at least 1.25L of DCM if you want to recover most of the GBL.

So a 0.5mol run (51.6g GABA), 0.5mol NaNO2 with 140ml of water was used. (this is as far back as you can go with reducing the volume of water--the total solution volume will be 200ml) 58.3g of 31.25% HCl was slowly dripped in with mag stirring (the addition must be done VERY slowly at first, to avoid the clouds of NO that you'd normally see).

After 24hrs of adding the last drop of HCl, 50ml of 31.25% HCl was added. The DCM extractions were cut back to 5x100ml--don't do this! The person should have used 5x125ml=625ml. Sure enough, the yield was slightly lower--31.6g crude (73%)--28.8g (67%) after atmospheric distillation.

25.2g of the distilled, acid-smelling, slightly-yellow GBL was taken and reacted with 24.6g NaHCO3 in 100ml water. It was refluxed for 30mins. There was a fishy amine smell to the mixture. BLECK. It was gross NaGHB that sane people shouldn't consume (but in the past, well, just read the caption under my nick). So 10ml of activated charcoal was added, the ~100ml was lightly boiled 5-10mins in a 600ml beaker with a stir bar. It was suction filtered over celite, and the charcoal and celite rinsed with about 15ml water two times. The result was some odorless NaGHB, the taste is MUCH improved. Of the 25.2g GBL used, 34.9g of NaGHB was produced (95%, i.e. 64% overall).

It was then boiled down to concentrate it, tucked away for a rainy day and not consumed. (how long will that hold true?)

I now strongly recommend for a work-up: solvent extraction, distillational, conversion to NaGHB, refluxing with activated charcoal and concentrating the solution before anyone even thinks about consuming the product. If you skip any of these steps you're taking unknown/insane health risks.
 
 
 
 
    Sifty
(Newbee)
10-02-03 00:16
No 462176
      Looking back     

I was re-reading through this gigantic thread and came across something that was never really followed up on.

In Post 402801 (M3Psych: "ascorbic acid", Chemistry Discourse):


It is well known that sodium ascorbate or ascorbic acid prevent the formation of nitrosamines (in vitro and in vivo). Would this be of use?

...

Aside from left-over solvent, unreacted H2SO4 (etc), the nitrosamines would be the only toxic compounds in this rxn so if ascorbic acid can be used the product after distillation should be nearly as pure as any (probably at least 99.8%).




Anyone got any input on this? Is this legitimate or crap? Since no one responded to it, I thought I'd re-ask his question and see if any bees had any insight.

-Sifty


"...Come with us and leave your earth behind..." - Chem.Bros.
 
 
 
 
    methyl_ethyl
(Hive Bee)
10-02-03 03:49
No 462216
User Picture 
      Sulfuric     

IMO the off taste/smell is not due to nitrosamines, I would believe that the H2SO4 would destroy any of the nitrosamines that may have been formed. 

Further reading:

Post 378237 (fierceness: "nitrosamines", Chemistry Discourse)

Post 412468 (hCiLdOdUeDn: "Nitrosamine decontamination", Chemistry Discourse)

I think ascorbic acid was initially what was used in the food industry to destroy N-Nitrosamines, I think HCL, or H2SO4 would do the trick just as well, just as long as you do not apply it to your morning bacon wink

     Unipolar Mania, It's good for life... laugh
 
 
 
 
    fierceness
(Hive Addict)
10-02-03 04:17
No 462220
      I think pretty much any acid will destroy the...     

I think pretty much any acid will destroy the nitrosamines.  I read texts of them using HCl, HBr, Vitamin-C, etc.

This is definitely good news about the activated charcoal.  Now, where was that guy who was going to run a GCMS on the product? wink
 
 
 
 
    foxy2
(Distinctive Doe)
10-13-03 03:07
No 464320
User Picture 
      If it is amine contamination I think they sell     

If it is amine contamination I think they sell Zeolites specifically for removing ammonia from fish tanks.  You might want to look into these as they might work better than activated carbon for getting out the fishy.


Zeolite

All natural Zeolite with exceptionally porous surface that allows the removal of ammonia, phosphates and heavy metals, main cause of elevated Ph in aquarium water. Ideal for use with Hydor Prime external filters or other filtering systems for fresh water and marine aquariums. Directions for use: before using, place zeolite in net and rinse in warm water to remove excess dust then place in filter.


 
 
 
 
    hester18
(Stranger)
11-04-03 04:54
No 468618
      Chemical Eq     

Do you have the balanced equations for that reaction? Im asking mainly because of the side reactions taking place and I am wondering what other products are formed?

~Hester18
 
 
 
 
    merbst
11-05-03 07:05
      Side reactions
(Rated as: misinforming)
    
 
 
 
    fierceness
(Hive Addict)
11-06-03 03:03
No 469023
      No Explosions     



Sodium Oxide:
http://ptcl.chem.ox.ac.uk/MSDS/SO/sodium_oxide.html
Reacts violently with water... haha, yes, if one were to attempt to distill the pre-DCM extracted reaction mixture, there would be many small to medium sized explosions at ~ 103C, as the sodium sulfate has precipitated, and is decomposing into SO2 which bubbles to the surface to react with the still humid flask interior.




There were no "explosions".  The first time this procedure was attempted, swif steam distilled (in situ) the post reaction mixture.    No explosions were noted.  However, this procedure has obviously been refined, so if you want to attempt it and (hopefully) use your analytical equipment to test it, go right ahead :)

 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
11-06-03 06:06
No 469059
      Merbst     

Merbst, all of your references do not apply to the conditions used in this synthesis. I won't bother expanding my point (it should be obvious to people with any more advanced knowledge of chemistry). Your post is misinforming on every point you make.
 
 
 
 
    merbst
(Stranger)
11-06-03 07:04
No 469066
      Re: Merbst, all of your references do not...     


Merbst, all of your references do not apply to the conditions used in this synthesis.



How so?  Care to provide any references for those of us without "advanced knowledge of chemistry" to learn from?
The question "Do you have the balanced equations for that reaction?" was asked, and I attempted to provide useful information to answer at least part of this question.
Chromic, would you like to provide a balanced equation for this reaction?
If my post is misinforming please elaborate what is misinforming about it so that you may actually contribute something useful.

 
 
 
 
    Antoncho
(Official Hive Translator)
11-06-03 08:29
No 469077
      Here's your equation:     

R-NH2 + NaNO2 + HCl __> R-OH + N2 + NaCl + H2O


And yes, Chromic is absolutely right - your post is wrong on pretty much everythingsmile


Antoncho


P.S. A question to everyone: does anyone have an idea as to how to isolate GABA from the pills?laugh Sounds not too much fun, but is nevertheless the only practical opportunity for SWIMcrazy

His plan is to take pills, crash them in IPA, filter out the starch/TiO2/Ca stearate etc. Then add H2SO4 and put into the freezer, hoping that GABA sulfate would come out.

The only problem is - SWIM hasn't a slightest idea how much GABA will dissolve in IPA - taking too much alcohol will result in incomplete xtallization, taking too little will result in extra H2SO4 forming acidic salt with GABA, which is very soluble and won't xtallize at all.


Can anyone help?frown
 
 
 
 
    merbst
(Stranger)
11-06-03 09:10
No 469082
      Thank you Antoncho for the equation!     

Thank you Antoncho for the equation!
Can anyone provide the equation if H2SO4 is used?
Does this mean that if HCl is used no NO will be evolved?
Obviously with H2SO4, there is no Cl available to create NaCl, thus a different salt of sodium is formed, what is this?
SWIM personally experienced "mini-explosions" at 103C while experimenting with distilling the (H2SO4) reaction mixture pre-DCM extraction, but did not post-DCM extraction.
I apologise for the misinforming nature of my post, I was only providing what I had read elsewhere, can anybody clarify what is incorrect about it?
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
11-06-03 23:21
No 469222
      Doesn't sound right.     

Antoncho, isolating GABA from pills is not as good of an idea as finding a source of the pure amino acid. How many times did I say it? Well, turns out I'm right. tongue (... there was a time where you complimented me for promptly admitting to my prior mistakes--only fitting that I gloat now, esp. after testing this for you)

Did you try the water test I mentioned? Maybe what's in the capsules is pure GABA. Solubility is 1g GABA/2ml H2O. I can get you better solubility data if you'd like (it's actually slightly more soluble, this # could maybe be 1g/1.5-2ml H2O).

Using TOO MUCH ipa is not a problem... simply distill down the IPA until you start to see the GABA ppt out.  However, solubility is WORSE than 1g/50ml IPA, how much worse--I don't know, but it doesn't look good (perhaps 200ml+ for one gram). Solubility is about 1g/100ml (maybe closer to 120ml) in MeOH. You can't ppt out the GABA by adding even just one drop of sulfuric acid (tried it). Perhaps using a mix of MeOH/water for the pill extraction if it's not pure GABA and the water extraction fails. (water extractions often work with non-GAKK pills) I think the reasoning behind this is that the GABA badly wants to form a Zwitterion.

But, then again, for all I know what I have could be NaGABA or GABA.HCl. Hmm! That's worth testing for... why not! It'll put your mind at rest.

Well, it's certianly not GABA.HCl, as it buffers sulfuric acid added to methyl orange. The results I get with phenolphthalein are confusing. NaOH will turn it pink at first, then as more NaOH dissolves, deep red. (falsely indicating that it could be NaGABA) But, back titrating it a red solution of NaOH/water with GABA turns it pink. I think that's because the pI of GABA 7.1 is close to the pKa of phenolphthalein, 9.4.. and just a little bit of pink shines thru at pH close to 8. (that's my educated guess) Plus if it was NaGABA, one eq of HCl would not have a chance to react with all the NaNO2, and I'd be seeing greatly reduced yields.

Merbst, those "mini-explosions" are what is called bumping... they are not any type of hazardous decomposition of any salt. Use a mag stirrer when distilling (and even that may be insufficient when large qty's of NaCl or Na2SO4 ppt'd out). Mods, please stop me! I really shouldn't answer these questions anymore! I'm about to _cry_ or _scream_. Take your questions to the Newbee forum.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
11-07-03 00:58
No 469246
      Side reactions     

Okay, Merbst, I think I've been a bit rash. There was one question in your post of good merit to this discussion.

The likely side reactions to this method are the production of gamma-chlorobutyric acid, gamma-(3-carboxypropoxy)butyric acid and pent-4-enoic acid. The toxicity of those chems is unknown. I wouldn't eat them if I were you. I'm pretty sure these side-reactions do not take place in good yield (but are definitely there in ppm and perhaps ppt), as the journal states 100% conversion to GBL/GHB.

This is why I still don't feel 100.000% comfortable writing a final writeup--and do not want anyone else to do so. We need someone with GC/MS to analyze the product before we put people's lives at risk. In fact, I'm feeling rather uncomfortable with this information even being on The Hive publically, but I have made several disclaimers throughout this thread. (this being YET ANOTHER disclaimer)

[addendum: I noticed this thread has exceeded 10,000 views... the knowledge is starting to get rather public and still no one reading this has access to a GC/MS?]
 
 
 
 
    fierceness
(Hive Addict)
11-07-03 20:49
No 469509
      GABA pills     

Antoncho:  Using pills as the source is only asking for trouble.  SWIF ran this reaction using capsules that said they were filled with pure GABA powder from a well known US nutrition chain store.  The powder would not even dissolve in water because they were mixed with some inactive unlisted ingredient.  If you get the stuff that is SUPPOSED to be mixed with water for consumption, your life will be a lot easier :) 

This reaction is the easiest reaction in the world to run and almost as easy to work up with simple distillation equipment.
 
 
 
 
    Antoncho
(Official Hive Translator)
11-08-03 12:18
No 469632
      Thanx a lot for the advice!     

Dear Chromic, - THANK YOU very much for the research you have done to make my life easiersmile



Now guys - i perfectly understand why you say that dealing with pills is categorically unadvisable... As a matter of fact, I hold that very same opinion as welllaugh.

However, it is one of Russia's sad realities that any reagent which has a structure more complicated than toluenesmile is prohibitively expensive - at least for a non-commercially oriented, and not very rich, for that matter, hobbyist kitchen chemist.
In other words, even if SWIM was able to locate a 'food-grade' GABA source (what purpose is it applied for in your parts of the world?), he doubts that he could afford buying a kilo of it.



Beesides, having a kilo of GHB - even potentially - is something that SWIM wants to avoid at all costslaugh SWIM already had a fortune of aqcuirinmg a kilo of 1,4-BDO... Which lasted about 3 months, 90% of the stuff being consumed by SWIM personally... (yeah, Placebo's method rules, esp. with Assholium's modification).
And he doesn't want to repeat this againsmile




As for isolation - well, it surely doesn't look that easy anymore... Possibly, crushing it out of an aqueous solution with IPA could work, who knows... In any case, the goal is only to get rid of the sugars. Isn't it really strange that GABA doesn't dissolve in alcohols? Whilst GHB, even in form of a sodium salt, dissolves readily... Weird.





Now - onto a totally different topic. I really think that there's a great room for improvement of this rxn.
 
1st of all, why not carry out diazotization at reduced temperature? That way, more HCl can bee added at a time - possibly, even all of it, since HNO2 holds much better in water at 5 С (the sources say that N2O3 boils at 3,5 C - so if the addition is done at that temp, there won't bee any nitrous fumes at all).

Lowering the temp will also slow down the formation of diazonium salt, but at the same time, the higher concentration of nitrous acid will probably compensate for that.

In any case, the rxn could bee periodically titrated for HNO2 consumtion (any ideas, what would bee an ideal titration reagent?)

The 2nd thought - why not use some copper salt for improving the decomposition of diazo compound?


Generally, i don't know a shit about diazotization of aliphatic amines, so all of the above is just rambling.

I wonder, however, why this rxn takes such a long time.

And i wonder yet more what is the rate-limiting step in this rxn - diazo salt formation or its decomposition?



Antoncho
 
 
 
 
    hester18
(Stranger)
11-08-03 17:11
No 469652
      Eq. and about NO and NO2     

Thanks for the Eq. but my next question is about the gases said to be produced, more importantly the more dangerous of the two, NO2. In the Eq. there is nitrogen produced but at what point are the other gases or gas produced. Ive seen the two gases used almost synonomously, which gas is produced and why? I see chromics initial workup on this thread mentions nitric oxide, and some other workups mention the 'insidious' brown NO2 gas if the acid is added too quickly. Are both these liberations of gases possible and if they are why are the different gases produced?
R-NH2 + NaNO2 + HCl => R-OH + N2 + NaCl + H2O
 
 
 
 
    fierceness
(Hive Addict)
11-09-03 02:38
No 469705
      swif's notes     



1st of all, why not carry out diazotization at reduced temperature? That way, more HCl can bee added at a time - possibly, even all of it, since HNO2 holds much better in water at 5 С (the sources say that N2O3 boils at 3,5 C - so if the addition is done at that temp, there won't bee any nitrous fumes at all).



SWIF always used an ice bath while adding the HCl, and just let the flask sit in it the whole 12-16 hours and let both come to RT gradually.  Otherwise, too many fumes were produced.

As for your suggestion on using a copper salt, swif never attempted that.  As for the reaction time, you can see that most of the bubbling happens in the first 6-8 hours, but you can definitely see more bubbling for the whole 12 hours (especially if you leave it in the ice/water bath and let both come to room temperature gradually).  All the GABA swif used was food grade -- the supplement is mixed with water and taken that way.

 
 
 
 
    Antoncho
(Official Hive Translator)
11-09-03 20:44
No 469825
      And i wonder yet more what is the ...     

And i wonder yet more what is the rate-limiting step in this rxn - diazo salt formation or its decomposition?


By saying this i meant that if the rate-limitin' stage is the decomposition, it would mean that by allowing the rxn proceed for 24hrs you actually allow all sorts of side-rxns to occur.

And, more importantly, the process may and should bee sped up.

I tried searching Espacenet for the patents concerning diazotization of aliphatic amines...

And that's what they say (in this proc they perform a one-pot hydrogenation of a fatty long-chain nitrile, followed by diazotization/hydrolysis):




Patent GB494666






So, as you can see, in their case the rxn proceeds pretty fast...

I wonder why it takes 14hrs in our case... Fierceness, are you positively sure that 14 hrs is absolutely necessary for all the nitrous to react?


Antoncho
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
11-09-03 22:09
No 469858
      At least!     

>Fierceness, are you positively sure that 14 hrs

At least 14 hours are needed. You can still see small bubbles of N2 forming 24hrs later.
 
 
 
 
    Antoncho
(Official Hive Translator)
11-10-03 00:51
No 469900
      Sorry for repeating this all over again, but...     

... but from what you guys both said it just wasn't entirely clear.

Is at least 14hrs needed for disappearance of nitrous fumes or for disappearance of nitrogen bubbles?

My point is - the rxn has two distinct phases: 1st, a diazonium salt is formed, 2nd, it gets hydrolysed to the alcohol.

Once the 1st stage is over - i.e., no NO2 is evolved, it makes sence to speed up the 2nd stage as much as possible - to prevent side-reactions.

OTOH, my textbooks say that in case of primary amines, the yields are usually low due to various rearrangements, so heating might not bee a good idea. But some cuprous salt will surely do what we want.


Please, clarifysmile


Antoncho

P.S. My pills turned out to bee absolutely unfilterable after dissolving in waterlaughlaughlaugh Fucklaugh
 
 
 
 
    fierceness
(Hive Addict)
11-11-03 03:20
No 470082
      reaction time     



Is at least 14hrs needed for disappearance of nitrous fumes or for disappearance of nitrogen bubbles?




You can see N2 bubbles for at LEAST 16 hours (lots at first, not as much later).  Perhaps it has something to do with the fact that it is in an ice/water bath the whole time.  You don't get much NOx fumes if you add the HCl/H2SO4 slowly and while the flask is in an ice bath.  Furthermore, if you do get the nasty green gas, it is only visible a maximum of 30 seconds after adding the portion of acid. 

SWIF cannot do this reaction anymore -- no time and no workspace.  However, in the 6 or 7 times he did it, he did in fact get good (albiet wrong-tasting) product.  He never tried the activated charcoal filtering or the copper salt. 

Antoncho-  sorry to hear about your pill drama!  SWIF was at that point too when he first attempted it.  Absolutely nothing would dissolve.  I take it ordering GABA online is out of the question?  Perhaps this rearrangement is what is causing the foul tasting impurity?

 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
11-11-03 05:54
No 470112
      Celite     

Did you try using celite to do the filtration? Also, did you try a 50:50 mix of methanol/water? (I'll get GABA solubility data if you find an alcohol:water mix that allows filtration with celite)

Btw, we did mean N2... the NOx gas is definitely brown not green. For whatever reason this reaction does happen in good yield with side-rxns at a minimum.
 
 
 
 
    placebo
(arrogant bee of the day)
11-11-03 09:07
No 470144
User Picture 
      I am sorry to go off-topic, but... Atoncho...     

I am sorry to go off-topic, but...
Atoncho...

SWIM already had a fortune of aqcuirinmg a kilo of 1,4-BDO... Which lasted about 3 months, 90% of the stuff being consumed by SWIM personally... (yeah, Placebo's method rules, esp. with Assholium's modification).



Thanks, it's nice to see someone finally tried it and with good results.
But, I am interested in this modification you speak of and have UTFSE to find it, but it seems it must be in Russian as I can't find it. Could you tell us about it, give us a link, start a new thread or PM me as not to hijack this thread?

Sorry again, please continue this interesting thread.


I'm not fat, I'm just too short for my weight.
http://www.whatreallyhappened.com
 
 
 
 
    fierceness
(Hive Addict)
11-11-03 18:41
No 470248
      this bee's limitations :)     



Did you try using celite to do the filtration? Also, did you try a 50:50 mix of methanol/water? (I'll get GABA solubility data if you find an alcohol:water mix that allows filtration with celite)




Nope, never tried it.



the NOx gas is definitely brown not green



Sorry, I'm colorblind :)  i got close enough, though :)

 
 
 
 
    shockwave
(Stranger)
11-12-03 22:19
No 470550
      Changes For Better Or For Worse???     

On the recent attempt, Swim changed some of the elements.

A. Swim switched over to reagent sulfuric from 95% Sulfuric.

B. Commerical NAOH from ACS.

C. Swim noticed that bubbles were present even after 12 hours (Swim never noticed before because of the color of impure sulfuric). Swim decided to heat the mixture and used the full 6 hours for the second sulfuric addition.

Results: 72% yield of weaker product

Swim contends that the second addition of sulfuric weakens the final product.

On Products That Were Produced:

A. Faster Synths Produced Stronger Side Effects (Numb Areas On The Forehead and On The Scalp)

B. Second Sulfuric Addition Produced Weaker Results (6 Hours Was Way Too Long)

C. Loss Of Strength After Product Sat (After Ph Phase, Product Loss Purity)

The best product was produced after 12-16 hours after last drop of sulfuric was dripped. Sulfuric was only allowed 2 hours to sit afterwards on second addition.

Product was salty

Distillation produced a smell of oil thickness kind of like popcorn oil.

Swim is going to try to reproduce the identical product to make sure it wasn't the ingriedients that caused a switch in purity and in taste from salty to bitter. Swim will isolate the final result and repost any updates.

Two things confuse me. Why would the a faster unsafe method produce better results? And why is everyone viewing this thread? I strongly suggest that people not try this or worse (try to mass produce). You will not get a final product that is outstanding at this point. Unless you are willing to experiment with chemical insanity and homeowner destruction, go order some ambien or something.
 
 
 
 
    shockwave
(Newbee)
11-25-03 03:46
No 472995
      Crystalization     

Has anyone encountered crystalization after the first sulfuric additon at cold temps? That happened on one simulation. In the final run, I think unreacted nitrite made its way into the crude. What steps are needed if that occurs and what should be done prevent it?
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
11-25-03 06:41
No 473028
      Volume     

If you're using ratios like 100g GABA, 66.9g NaNO2, 230ml water and with 26.4ml H2SO4... you'll see that the 69g Na2SO4 that forms actually needs 248ml water to dissolve in (and mind you this is at room temp, solubility is likely a touch lower at cold temps)... so at the end of the day, you'll see a precipitate of Na2SO4 that forms after the first addition. I've never personally seen this, but it means nothing should it happen to you... if it's happening with more dilute solutions, I've never seen it and shouldn't expect it.

If that is the source of your "problem" you can go back to HCl (because NaCl has a higher solubility per mol Na, ie 57g NaCl would be formed only requiring a solution volume of 159ml to dissolve it--mind you the reason you can't go below about 230ml water is because GABA/NaNO2 require that much water to dissolve in) or just ignore the "problem". (i.e. it's not a problem)
 
 
 
 
    silenziox
(Hive Bee)
11-25-03 07:57
No 473035
      lab test     

Has anyone tested is the final product gamma-BL or beta-BL?

www.badgerbadgerbadger.com
 
 
 
 
    shockwave
(Newbee)
12-07-03 21:25
No 475257
      Success Applied     

While trying to figure out how to maximize the yield, Swim stumbled on to a couple of interesting things.

A. Sulfuric should only stay in for 2 hours with no assistance on the second addition. When the sulfuric was allowed over 2 hours, distilling and seperation took twice as long. Also, the positive effects only lasted half as long. This was tested 5 times with two different subjects.

B. The RXN should sit for 24 hours without any tampering before the second sulfuric addition.

C. The activated charcoal technique should be written up to apply to gbl and NA-Ghb without a vacuum source. It was almost impossible to filter out the gunk normally.

D. It is almost impossible to distill fully without a vacuum source. Swim has tried and failed. But then again others may have had more success.

With these under consideration, yield is 70% for swim and it takes around 30 hours.

Thanks Chromic and Fierceness For The Great Foundation and All The Help

PS: Still trying to stop rate of decay of gbl. Swim has tried storing the gbl in a cooled environment, room temps, and warm temps. Also, Swim has tried seperating the gbl in different containers. If anyone has any advice, please feel free to offer.

smile
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
12-07-03 23:57
No 475278
      Don't drink it if you can't distill it!!!     

>It is almost impossible to distill fully without a vacuum source.
>Swim has tried and failed. But then again others may have had more success.

DON'T CONSUME THE GBL IF YOU CAN'T DISTILL IT!

At the very least use a steam distillation. Slowly drip in water as you distill the mixture (10ml water for every 1ml GBL).

Distillation at atmospheric pressure is totally possible. You need to insulate everything with glass wool otherwise you'll get too much reflux.. (even before clamping the flask). Make sure to quickly remove the heat source once the flask starts to empty or you'll burn your stir bar. To remove the crap that remains in the flask, first let it cool, add water, scrub as best as you can, and use diluted bleach (allow it to sit about 6hrs) to remove the last of the stains.
 
 
 
 
    shockwave
(Newbee)
12-10-03 18:47
No 475975
      Cold Seperation     

Swim tried to gauge yield of a steam distill of crude gbl. Swim found the best way to this is to freeze the end product. Swim found that he still lost 40% on this distill. Swim will try again. On a side note, Swim experienced SOX on the second addition which he had not seen before. He believed it was caused by a shorter duration between the sulfuric additions. Then swim believed it was caused by heating or cooling the rxn. In the end, it was caused by excess stirring. Swim has timed the process for 3 hour drip, 14 hour wait (heated and very little stirring), 2 hour wait on the second sulfuric addition, 30 min seperation and a 25 min distill. Of course, this is not to be attempted. Swim wanted to know if there is anyway to do a cold seperation of the gbl from crude. I'm not sure this is possible.

smile

Edit: Swim will try cooling and a sealed lag grade flask to stop gbl decay. Not sure if the gas experienced was SOX. It was brownish similar to that expereinced on a fast drip. Thanks Chromic tongue
 
 
 
 
    fierceness
(Hive Addict)
12-10-03 21:00
No 475994
      no.. distillation is an absolute necessity...     

no.. distillation is an absolute necessity (along with solvent extraction).. in fact, until someone with access to analytical equipment tests the results from this method, I suggest that you do not take any shortcuts..
 
 
 
 
    hester18
(Stranger)
12-11-03 02:33
No 476039
      How would the gas SOX be formed in the reaction?     

If the gas was brown it was most likely the deadly NO2 gas,
SOX or SO2 (most probable) is colorless.
I think the smell would easily determine if it was a sulfur containing compound or a nitrogen containing compound, if it gave a suffocating, choking odor...or in the case of the NO2 you probably wouldnt have been able to post if you had gotten a whif.
~Hester
 
 
 
 
    shockwave
(Newbee)
12-11-03 04:45
No 476058
      Weird Reactions     

Not sure how it occured. The only constant was the amount of stirring. The properties of the rxn also seems to help. Usually a good batch will be a light green or yellow before the second addition. But the gas that rose was troubling. Yield decreased by 25%. Distill and seperation rose by 25%. The gas was similar to gas released from a fast drip. I believe it is SOX because of its color, reaction, and heat. The flask even changed color.

Fierceness: Didn't mean seperation of DCM from GBL. Just a freeze of crude gbl into pure gbl. Not sure if that is even possible. Maybe filtering that with activate charcoal. Swim just loses a significant portion in a steam distill.

Edit: Hester I think you are correct on the gas. Just puzzling about the gas being so late into reaction. Anyways... back to studying for finals tongue
 
 
 
 
    Rhodium
(Chief Bee)
12-17-03 21:30
No 477462
User Picture 
      Hydrolytic Nitrosation of Amino Acids with NaNO2
(Rated as: excellent)
    

As mentioned in Post 455610 (StraightEdge: "Reactant: 4-amino-butyric acid Products: ...", Chemistry Discourse)

Hydrolytic Nitrosation of Amino Acids with Sodium Nitrite:
GABA -> GBL (30%) and GABA Methyl Ester -> GBL (80%)

Jean-Paul Gouesnard
Bull. Soc. Chim. Fr. (1) 88-94 (1989) (https://www.rhodium.ws/pdf/gaba2gbl.pdf)

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    merbst
(Stranger)
12-21-03 06:28
No 478136
      Recrystallizing calcium or magnesium GHB     

To purify further, consider recrystallizing the GHB as a calcium or magnesium salt.  This is done using calcium hydroxide, magnesium hydroxide, or magnesium carbonate.
ABSTRACT: A method for the production of nonhygroscopic magnesium and/or calcium
salts of 4-hydroxybutyric acid. A member of the group consisting of magnesium hydroxide, magnesium oxide, magnesium carbonate, calcium hydroxide, calcium oxide and calcium carbonate is reacted with 4-hydroxybutyric acid and/or gamma- butyrolactone in an aqueous solution. The solution is crystallized at a sufficiently low temperature for producing a solid nonhygroscopic salt. Waterfree calcium 4-hydroxybutyrate and waterfree as well as hydrated magnesium hydroxybutyrate are added to pharmaceutically acceptable carrier or filler material for production of tranquilizing and/or sleeping drugs.

How well would this be able to purify in lieu of distillation?

Patent US4393236 courtesy of young Rhodium!
http://www.lycaeum.org/forums/alchemy/Messages/316.html
 
 
 
 
    M3Psych
(Newbee)
02-09-04 19:58
No 487506
      Trying to revive this thread... 1.     

Trying to revive this thread...

1. Problems w/ NO -- Couldn't the resulting NO be bubbled through H2O or IPA? Since it's 7.8% soluble in H20 at 0C (http://www.camd.lsu.edu/msds/n/nitric_oxide.htm) would this be an effective "trap" for the NO, or would something like IPA be a better choice?

2. Discoloration/taste -- Has anyone pH tested the final product? Has anyone used ACS or FCC grade reagents? Has anyone tried boiling the GHB w/ activated charcoal? The sour taste sounds like it's too acidic, and the discoloration could be from OTC reagents.
 
 
 
 
    shockwave
(Newbee)
02-10-04 02:10
No 487573
      Reagent NAOH     

I use to use reagent naoh but then again I never had an issue with the taste and it wasn't going to be a center piece smile

EDIT: I think the correct ph when diluted is around a ph of 2.5... Ph should be around 7.5
 
 
 
 
    shockwave
(Newbee)
02-10-04 02:13
No 487575
      NO2     

I'm not sure (any chemists please correct) but you can vent safely if you are talking about the drip procedure or afterwards. If you use an inlet adapter with ground fittings on the dropper funnel and flask.

EDIT: I think it's NO2
 
 
 
 
    M3Psych
(Newbee)
02-10-04 16:01
No 487698
      Reading about NO2 I could find nothing ...     

Reading about NO2 I could find nothing indicating that it's a "deadly gas" as was previously stated in this thread. The worst I found was that it was a respiratory irritant which is relatively commonly encountered (home heaters), although obviously not in the concentrations which would be found in the GABA -> Gxx synth.

I can't believe that NO ONE here has access to any analysis equipment...
 
 
 
 
    bouncer
(Stranger)
02-21-04 02:28
No 490081
      Its been almost a year since the post about...     

Its been almost a year since the post about making GBL from GABA and my question is - did the whole procedure "got better" in terms of quality of conversion and is it safe enough to use after conversion?
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
02-24-04 05:03
No 490744
      safe enough     

It's one year later and I'm still alive, so the product certainly isn't acutely toxic. Do make sure to do a solvent extraction with a distillation... and do clean it up with activated charcoal... you should be okay. Don't distribute to others until you know that what you're making is rather clean...
 
 
 
 
    shockwave
(Newbee)
02-28-04 23:23
No 491677
      Helping Swim     

I'm trying to help Swim. He doesn't have anyway to fully distill and no vacuum source for filtration and full distill. Swim does have activated charcoal but no complex filtration methods (just a funnel from what I could understand). Any advice?

EDIT: No activated carbon also, just filter paper
 
 
 
 
    shockwave
(Newbee)
02-28-04 23:25
No 491678
      Another Question     

Is it always required for the second sulfuric addition? On different scenarios, if the synth is let to sit for a long time... it seems a bit redundant but then again I'm not sure if it's for yield or quality or both.
 
 
 
 
    Sangreal
(Stranger)
02-29-04 06:01
No 491720
      it shouldnt be that hard to make your own...     

it shouldnt be that hard to make your own distillation setup, hell people have been distilling for thousands of years.  Fractional distillation is even possible by wrapping up a glass tube with aluminum foil to promote multiple distillations.  Take your sample and slowly heat it, attach the glass tube wrapepd with foil to it.  Then have a heartshaped piece attached to this at the top.  It should be able to send the vapor up, it'll condense on the sides and drip down.  If you want you can distill this product that you collect (your distllate) a few more times to increase purity and dispose of your pot resiude (the stuff in the bottom of your vial.  Would it be that hard to setup vacuum distillation with a couple flasks, a hirsch funnel, some good filter paper, some vaccum tubing, connect that to your sink to create negative pressure.  just my thoughts.
 
 
 
 
    shockwave
(Newbee)
02-29-04 08:04
No 491733
      True but     

Distilling is the easy part... I was a little vague in my post about swim's issues. Swim can't do a full distill. Swim can distill off all the dcm. But Swim can't distill the gbl after that. Even with steam distillation and all the methods that were described. Swim ends up with what he would desribe as a black liquid.
 
 
 
 
    merbst
(Hive Bee)
03-01-04 18:57
No 492037
      Toxins     

Both NO and NO2 are produced as toxic byproducts of this procedure.  The synthesis generates NO which reacts spontaneously with the O2 in the atmosphere to create NO2, and trace N2O5.  If you want to scare the shit out of yourself read this post: http://groups.google.com/groups?q=no2+poison+ppm&hl=en&lr=&ie=UTF-8&oe=UTF-8&selm=48l67b%244kk%40sulu.cldc.howard.edu&rnum=4
Bubbling through H2O is not enough, but bubbling through a tall column of H20/H2SO4 (high molarity) will convert most the gasses into Sodium Nitrite (aq).  Of course you would need to place a chemical resistant pump either in between the exhaust outlet of the addition reaction and the gas trap column, or at the exhaust of the gas trap column (preferred but difficult to engineer).  You also would need to leave enough room at the top of the gas trap column so that the bubbles coming up however many feet wont overflow out its exhaust.  You still shouldn't breathe the exhaust of course.

Nobody has replied to my suggestion about the feasability of recrystallization as the Calcium or Magnesium salt... Think about it, recrystallization is used to make almost every other product more pure, why shouldn't it apply here?

Based on everybody's description of the rancid smell, and the structure shared by GABA and GBL, it sounds like one of the major impurities is Butyric Acid. http://ptcl.chem.ox.ac.uk/MSDS/BU/butyric_acid.html
Possible impurities from the HCl addition to GABA have been described, would anybody care to describe any H2SO4 products?
Thanks
 
 
 
 
    Vitus_Verdegast
(Hive Addict)
03-01-04 19:09
No 492040
User Picture 
      Correction!     

Bubbling through H2O is not enough, but bubbling through a tall column of H20/H2SO4 (high molarity) will convert most the gasses into Sodium Nitrite (aq).

You mean a concentrated NaOH solution of course!

http://www.movieconnection.it/schede/nosferatu.jpg
 
 
 
 
    shockwave
(Hive Bee)
03-02-04 00:09
No 492146
      Very Interestin Merbst     

So.. would it be feasable to use the side reaction for Nos (it would be great to get two synths going for the price of one)? And I looked at the salt suggestion but it looked very complex.
 
 
 
 
    fierceness
(Hive Addict)
03-03-04 01:51
No 492533
      recrystallization     

SWIF tried to recrystallize the NaGHB solid from ethanol.  The solid is so hygroscopic though, that in my humid climate it makes it very hard to perform a proper recrystallization.  Either way, the product he was left with still had a foul taste.  This was before it was suggested to boil with activated charcoal though.

Someone give the activated charcoal and recrystallization a try!  And analyze your results!  This thread has been alive for so long, and it's such an easy synth.
 
 
 
 
    shockwave
(Hive Bee)
03-03-04 18:38
No 492703
      recrystallization help     

You need the salts in conjunction with the end product of the synth? I'm a little confused on this issue. It sounds like you combine the 2 elements and attempt to harvest the crystals. If anyone had some detail on this subject, I wouldn't mind trying this.
 
 
 
 
    merbst
(Hive Bee)
03-04-04 08:02
No 492902
      Vitus: Thank you, my bad, I meant NaOH.     

Vitus: Thank you, my bad, I meant NaOH.  Lo Siento Mucho!
Shockwave: if by Nos you mean NitrOUS Oxide, you are horribly wrong.  The side reaction produces NitrIC oxide, which is a horribly deadly gas.
 
 
 
 
    shockwave
(Hive Bee)
03-05-04 17:27
No 493186
      Whoops     

Sorry, my chemical knowledge is obviously lacking. I would still like any help anyone has to offer on the crystalization. I've pretty much perfected every other part of the process.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
03-28-04 05:57
No 497817
      GC     

I got a friend to run a GC on the distillate. It doesn't look terribly pure... a writeup is in the works. I'll post the results as time permits.
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
03-29-04 06:23
No 497944
      GC results     

Okay, the following is the retention time (in minutes) and area of the peaks (in %) I rewrote this by hand, there may be a small mistake in the areas as they don't add up exactly to 100.00000%:

1.538 0.00507
1.585 3.43322
1.609 71.79745
1.720 0.01006
1.786 0.00851
1.846 0.05474
2.034 0.00069
2.126 0.00500
2.280 0.00065
2.331 0.09253
2.435 0.77343
2.526 0.07623
2.801 22.92439
3.298 0.13063
3.365 0.00131
3.415 0.00496
3.499 0.00616
3.544 0.37968
3.808 0.00906
3.980 0.00500
4.182 0.00573
4.661 0.00361
4.910 0.02064
5.042 0.01892
5.150 0.03833
5.392 0.00111
5.668 0.01543
5.757 0.00276
5.815 0.00140
7.287 0.01222
8.839 0.16111

The 2.801 is the GBL, the 1.609 is the solvent that the sample was prepared in. My guess is that 8.839 or 3.544 could be GHB. 2.435 could be water. (any inputs? GCMS? SURELY you must have some ideas here, GC output is totally new to me)

Anyways, this means that the GBL made by distillation certainly isn't better than 95% pure. It is likely at least 2% contaminated. Treating with activated charcoal is absolutely necessary!!!

I'd like to run a GC/MS and may, as time permits. Analyzing the data however is not my strong suit.
 
 
 
 
    fawaka
(Stranger)
03-29-04 23:26
No 498018
      I think we owe you one.     

I think we owe you one.
It seemed everyone was waiting until someone had access to a GC/MS.
Lots of success with the MS!

None are more hopelessly enslaved than those who falsely believe they are free.
 
 
 
 
    fierceness
(Hive Addict)
03-31-04 05:45
No 498230
      Finally some progress! :)     

Finally, some progress!  Thanks Chromic.

Do you think these higher-percentage impurities could be the rearrangement product suggested in either this thread or the other related thread by me, or maybe gamma-butyric acid?

God I hope they aren't the dreaded nitrosamines!
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
03-31-04 11:01
No 498258
      other products     

>Do you think these higher-percentage impurities could be the rearrangement
>product suggested in either this thread or the other related thread by me,
>or maybe gamma-butyric acid?

I take it you mean butyric acid (other than the carboxylic acid group, it's saturated with hydrogen--no need for alpha/beta/gamma/etc). Could be. I sure hope it is.

There's no real way to tell until I can get MS results for each peak (even then, MS isn't my strong suit, so trying to identify the peaks will be a challenge in itself). I was hoping someone here would know something about GC and be able to tell me a bit of qualitative meaning to the results that I posted. GC/MS is harder for me to obtain.
 
 
 
 
    moo
(Hive Bee)
03-31-04 16:26
No 498311
      Butyric acid should stink to high heavens.     

Butyric acid should stink to high heavens.

fear fear hate hate
 
 
 
 
    foxy2
(Fragile ego)
04-03-04 02:57
No 498785
      A solvent blank, authentic gbl, thf, ...     

A solvent blank, authentic gbl, thf, 1,4-butanediol, GABA and ghb for comparison would really help to see whats going on.  Since these could all bee likely contaminants of the products.wink

If he still has access to the the GC, running the samples I mentioned MIGHT tell you alot, or it might not.smile

http://www.democracynow.org/ - The Exception to the Rulers
 
 
 
 
    methyl_ethyl
(Guardian)
04-03-04 04:57
No 498799
User Picture 
      Hmmmm.     

Very interesting Chromic, first off I do not know much about GC.  First question, why do you think that it is the solvent that "eluted" (if that is the right word) at 1.609min? What solvent did you use as a diluent?  I could of sworn that GBL resolved at ~1.6xx minutes (under DEA  reported "normal GC conditions", don't remember exactly off hand).  Also GHB would more than likely convert to GBL under the "normal" column temps associated with GC AFAIK, so I doubt it would elute seperately.

I Agree mostly with Foxy, the more samples you could run the better, A solvent blank, GBL standard, any volatile components that may end up in the mix could be analysed seperately also.  The more peaks that can be eliminated through "deductive reasoning" the better.  GABA might be better off analyzed by HPLC.  I am sure there is some of that in the mix... 

Well those are my thoughts, hopefully someone with some true analytical experience will comment....

regards,

m_e

     Unipolar Mania, It's good for life... laugh
 
 
 
 
    jsorex
(Hive Addict)
04-07-04 22:00
No 499581
User Picture 
      f     



This following DEA site has the GC/MS, FTIR/ATR, GC/FTIRD, NMR, and Quantitation by GC/FID.


1,4-Butanediol (BD) - Forensic Profile

http://www.usdoj.gov/dea/programs/forensicsci/microgram/journal_v1/mjournal_v1_pg7.html

gaba:

http://www.hort.purdue.edu/rhodcv/hort640c/methods/botl.htm

033102beer_1_prv.gif
 
 
 
 
    Rhodium
(Chief Bee)
04-08-04 02:11
No 499623
User Picture 
      Forensic Analysis of GHB, GBL & others
(Rated as: good read)
    

Forensic Analysis of gamma-Hydroxybutyric Acid, gamma-Hydroxybutyrate, gamma-Butyrolactone, and Related Compounds
Microgram Bulletin, Vol 37, No 3, pp. 52-55 (2004) (https://www.rhodium.ws/chemistry/ghb.forensic.html)

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Rhodium
(Chief Bee)
04-08-04 18:09
No 499751
User Picture 
      Extraction of GHB acid from aqueous solutions
(Rated as: excellent)
    

The extraction and infrared identification of gamma-hydroxybutyric acid (GHB) from aqueous solutions
Chappell JS, Meyn AW, Ngim KK
Journal of Forensic Sciences 49(1), 1-8 (2004) (https://www.rhodium.ws/pdf/forensic/ghb.aqueous.extraction.pdf)

Abstract
The chemical analysis of gamma-hydroxybutyric acid (GHB) in most forensic laboratories is complicated by the highly polar nature of the GHB molecule, which makes it unsuitable for direct analysis by gas chromatography (GC). Consequently, a popular analytical approach is to convert GHB into the corresponding lactone or a derivative compound that is then identified by mass spectrometry employed in conjunction with GC (GC/MS). An alternative approach is presented here where GHB may be isolated as a free acid specie from complex aqueous solutions employing a liquid–liquid extraction technique. This approach can yield a relatively pure residue of GHB that presents an infrared transmission spectrum that is sufficiently distinct for identification purposes. Infrared spectroscopy (IR) is a very popular technique that is available to most crime laboratories. The liquid–liquid extraction behavior of GHB is examined in detail and the uniqueness of the infrared spectrum is discussed.



Spontaneous Formation of gamma-Hydroxybutyric Acid in Tap Water Solutions of gamma-Butyrolactone
Per Lundquist, M. Jonsson and Johan Dahlén
Forensic Science International 136 (Suppl. 1), p 88 (2003)

Introduction:
In February 2002, gamma-hydroxybutyric acid (GHB) was classified by the Swedish authorities, while gamma-butyrolactone (GBL), the lactonic form of GHB, is still not admitted with any restrictions. Since GBL spontaneously is converted to GHB in acidic as well as alkaline solutions the present regulations cause problems for the forensic chemist. Although it is well known that a chemical equilibrium is established with the proportions 2:1 (GBL:GHB), less is known about the kinetics and how it is affected by the sample matrix. The sodium salt of gamma-hydroxybutyrate is normally produced illegally by mixing GBL and sodium hydroxide. When the base is added GHB is deprotonated and more GBL will be converted to GHB. This continues until all GBL has been consumed or until pH is below pKa (4.72) of GHB. The equilibrium discussed above theoretically means that about 33% GHB would form in aquatic solutions of GBL. Addition of a strong base, which is the typical approach used in illicit manufacturing, will increase the amount of formed GHB. It is, however, unknown to what extent other species, like those present in tap water, will affect the equilibrium and/or the kinetics of the reaction.
In the present work the extent and kinetics of the formation of GHB in GBL solutions of different types of Swedish tap waters were studied. A first aim was to evaluate whether it is possible to obtain a concentration of GHB that exceeds 33 % without addition of a base. A second aim was to study the kinetics to get an idea of the speed of conversion in different typical tap waters. This information is useful since the time between seizure and analysis may be several days.

Experimental:
Deionized water and water from seven different water plants (i.e. tap water) from the north to the south of Sweden was collected. The choice was based on principal component analysis (PCA) modelling of water quality parameters of 373 water plants and it was made with the aim to represent the different types of tap water available in Sweden as well as possible. GBL solutions with concentrations 0 (blank), 5, 25 and 50% were prepared for each of these waters. The solutions were stored at room temperature and the formation of GHB was studied as a function of time during 9 months. The GHB analyses were made using a capillary zone electrophoresis (CZE) method using indirect UV detection at 220 nm. The carrier electrolyte consisted of benzoic acid to allow for the indirect detection, tetradecyltrimethylammoniumbromide (TTAB) to reverse the electroosmotic flow and a tris buffer to maintain pH at 8.1. The samples were injected hydrodynamically. The method was such that no GBL was converted to GHB during the analysis.

Results:
Equilibrium was reached after 50-280 days depending on the type of water and the GBL concentration. Traces of GHB could be detected already after one day and after two days up to 0.8% GHB had been formed. Somewhat surprisingly, it was found that the kinetics was faster in deionized water than in all of the tap waters. As an example, 20% of the GBL (25% GBL in deionized water) had been converted to GHB after only 18 days. In general, the conversion was faster in the 25% solutions, followed by the 5 %and the 50% solutions. Two of the tap water samples showed conversion rates that were considerable lower as compared to those of the other waters. These samples had higher conductivity, alkalinity and total hardness than the other tap waters. The level of GHB at the equilibrium did not significantly exceed the expected 33%, which strongly indicates that a higher GHB concentration can not be obtained without altering the composition of the tap waters (e.g. addition of a strong base like sodium hydroxide).

Conclusions:
The type of water into which GBL is dissolved strongly affects the rate of GHB formation. Slower formation was found for tap waters with high conductivity, alkalinity and total hardness. Traces of GHB could be detected already after one day, which is important to have in mind, especially in countries where GHB is a controlled substance, while GBL is not. In all cases equilibrium was reached at approximately 33% GHB. This strongly indicates that higher GHB concentrations can not be obtained without altering the composition of the water, for example by the addition of a strong base like sodium hydroxide.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
04-12-04 02:44
No 500292
      Extracting with IPA     

Does anyone think that trying to extract with IPA might be a better solvent than DCM? (IPA and saturated solutions of NaCl aren't usually miscible)
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
04-13-04 19:31
No 500627
      Extracting with IPA     

IPA extractions won't work very well, IPA carries along too many salts (although it does seem to extract the GBL quite well).

I found that 99% IPA will actually remove water from a solution of brine. Pretty cool, but kinda annoying in this situation. (if anyone wants to try this extraction for themselves, prepare the IPA used to extract by taking 70% IPA and saturating with NaCl... then use the upper layer to extract from the saturated NaCl rxn mixture)

I guess I'd still love to try chloroform and EtOAc (as I suspect they'd be better solvents) before I publish the document, but I don't have a large quantity of either handy (my guess is that they're more rare for most other bees as well). Expect a write up very soon.
 
 
 
 
    pericles
(Newbee)
04-13-04 23:05
No 500674
      Chloroform     

If you weren't aware, chloroform is extremely easy to prepare via https://www.rhodium.ws/chemistry/chloroform.html. I can't comment on the quality of the resultant reagent, but it seems like distilation followed by a wash with water (as the chloroform / acetone boiling points are sort of close) should give you something of reasonable quality.
 
 
 
 
    Rhodium
(Chief Bee)
04-14-04 00:38
No 500695
User Picture 
      The article is now online     

I have now updated Post 499751 (Rhodium: "Extraction of GHB acid from aqueous solutions", Chemistry Discourse) with a link to the full-text article. Have a good read!

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Rhodium
(Chief Bee)
04-21-04 15:57
No 502061
User Picture 
      Metal analysis of GHB (and ephedrine)
(Rated as: good read)
    

Application of Inductively Coupled Plasma Atomic Emission and Mass Spectrometry to Forensic Analysis of Sodium Gamma Hydroxy Butyrate and Ephedrine Hydrochloride
Karen A. Wolnik, Douglas T. Heitkemper, John B. Crowe, Barbara S. Barnes and Thomas W. Brueggemeyer
Journal of Analytical and Atomic Spectrometry 10, 177-181 (1995) (https://www.rhodium.ws/pdf/forensic/ghb.metal.analysis.pdf)

Abstract
The identity and relative amounts of various elements in samples of two compounds, sodium gamma hydroxy butyrate (GHB) and ephedrine hydrochloride (ephedrine), have been used to compare items of evidence. GHB, unapproved for use in the United States, and ephedrine, used in the illicit manufacture of methamphetamine, are currently of interest to law enforcement authorities. In this paper, the analysis of the elemental impurities in GHB by inductively coupled plasma atomic emission spectrometry. (ICP-AES) has been used to further the investigation of clandestine manufacturing sources. The following elements were detected in samples of GHB: Ba, Ca, Cd, Fe, K, Mg, Ni, P, Pb, Si, Sr, and Zn. Results were used to demonstrate an association between samples of unknown origin. Analysis of samples of ephedrine of known origin from legitimate manufacturers by ICP-mass spectrometry showed that Al, Ba, Mn, Pt, Rb, and Sr were the most useful for discriminating between sources and making direct comparisons. Interpretation of results with respect to the intended use of conclusions derived from those results is discussed.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Rhodium
(Chief Bee)
07-02-04 21:36
No 517022
User Picture 
      The chemical interconversion of GHB and GBL
(Rated as: excellent)
    

The chemical interconversion of GHB and GBL: forensic issues and implications
Laura A. Ciolino, Mantai Z. Mesmer, R. Duane Satzger, A. Caroline Machal, Heather A. McCauley, and Angie S. Mohrhaus
Journal of Forensic Sciences 46(6), 1315-1322 (2001) (https://www.rhodium.ws/pdf/forensic/1992-2001/ghb-gbl.interconversion.forensic.issues.pdf)

Abstract: In this work, the interconversion of GHB and GBL in a variety of aqueous media was studied. The effects of solution pH and time were determined by spiking GHB or GBL into pure water and buffered aqueous solutions, and determining the GHB and GBL contents at various time intervals. The degree of GBL hydrolysis to GHB was determined for several commercial aqueous-based GBL products, and further studied as a function of time. The effects of temperature and time were also determined for five commercial beverages spiked with GHB or GBL. GHB and GBL contents were determined using high performance liquid chromatography (HPLC). GHB and/or GBL confirmations were made using gas chromatography-mass spectrometry (GC-MS) and/or infrared spectroscopy (IR).

Solution pH, time, and storage temperature were determined to be important factors affecting the rate and extent of GBL hydrolysis to GHB. Under strongly alkaline conditions (pH 12.0), GBL was completely converted to GHB within minutes. In pure water, GBL reacted to form an equilibrium mixture comprising ca. 2:1 GBL:GHB over a period of months. This same equilibrium mixture was established from either GHB or GBL in strongly acidic solution (pH 2.0) within days. A substantial portion of GBL (ca. 50%) was hydrolyzed to GHB in aqueous-based GBL products, and in spiked commercial beverages, after ambient storage for a period ranging from several weeks to several months. Heat increased and refrigeration decreased the rate of GBL hydrolysis relative to ambient conditions. These studies show that hydrolysis of GBL to GHB does occur in aqueous-based solutions, with samples and time frames that are relevant to forensic testing. Implications for forensic testing and recommendations are discussed.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Rhodium
(Chief Bee)
07-02-04 22:16
No 517032
User Picture 
      Color Test for GHB using NH4OH/Fe(III)
(Rated as: excellent)
    

Rapid colorimetric screening test for γ-hydroxybutyric acid (liquid X) in human urine
William C. Alston and Karno Ng
Forensic Science International 126(2), 114-117 (2002) (https://www.rhodium.ws/pdf/forensic/ghb-gbl.colortest.pdf)

Abstract
A rapid colorimetric test for the detection of γ-hydroxybutyric acid (GHB) is described. The ferric hydroxamate test for ester detection has been adapted to detect GHB in human urine samples from a healthy female and a healthy male subject. The assay can be performed within 5 min and with a GHB detection limit of 0.5 mg/ml when 0.3 ml of human urine is used and a GHB detection limit of 0.1 mg/ml when 1 ml of human urine is used. The colored complex indicating the presence of GHB is purple according to the assay conditions. Test results are free from the interference by alcohol, phenolic compounds and other biological chemicals under the assay conditions. In addition, the colorimetric test is free from the potential false-positive test result that could result from physiological concentrations of GHB.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    armageddon
(Hive Bee)
07-06-04 20:13
No 517795
      lactone purification     

I once read in a patent that GBL can be purified by forming a phenylhydrazone (think it was 2,4-dinitro-phenylhydrazone..) which can then conveniently be recrystallized... (think I remember reading that something like "yellow needles" was said, but not sure about it)

- and unfortunately I am unable to relocate this useful bit of info... crazy

But hey, can't lactones - like most ketones - be purified via the oxime (or maybe bisulf)? (just an idea)

Greetz A

"..ein Trank von unterschiedlicher Farbe, in ihm ist Heilung für die Menschen."
 
 
 
 
    Rhodium
(Chief Bee)
07-06-04 21:53
No 517808
User Picture 
      How about some afterthought?     

I once read in a patent that GBL can be purified by forming a phenylhydrazone (think it was 2,4-dinitro-phenylhydrazone..) which can then conveniently be recrystallized...

But as the molecular weight of butyrolactone is 86 g/mol and that of 2,4-dinitrophenylhydrazine is 198, it means that you would  need to use ~2.75 kilos of the hydrazine to purify one liter of GBL. Rather absurd if you ask me, especially considering its cost.

But hey, can't lactones - like most ketones - be purified via the oxime (or maybe bisulf)? (just an idea)

But hey, lactones are esters, not ketones...

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    armageddon
(Hive Bee)
07-06-04 22:28
No 517816
      Well, I didn't think that far...     

Well, I didn't think that far... (2,4-dinitrophenylhydrazine is priced at ~120 bucks / 500g (ACROS) - this way of purifying is probably more suited for preparing analytical samples than for preparative work on big scale laugh)

But hey, gamma-butyrolactone is also called tetrahydrofuranone - so the ending "-one" doesn't stand for ketones? (funny - and the C=O in esters behaves different from carbonyl groups in ketones due to extra oxygen atom present - did I get that right?)

(sorry for my lack of afterthought)

A

"..ein Trank von unterschiedlicher Farbe, in ihm ist Heilung für die Menschen."
 
 
 
 
    Rhodium
(Chief Bee)
07-06-04 23:20
No 517832
User Picture 
      Nomenclature and carbonyl surroundings     

But hey, gamma-butyrolactone is also called tetrahydrofuranone - so the ending "-one" doesn't stand for ketones?

I'd say that the "-one" suffix is rather an indication of the carbonyl group "C=O" being present. By looking at it that way, all nomenclature is consistent, but you still have to evaluate the chemical structure to find out if you have a ketone (as in 2-propanone) an ester (as in tetrahydrofuranone) or an amide (as in pyrrolidinone).

(funny - and the C=O in esters behaves different from carbonyl groups in ketones due to extra oxygen atom present - did I get that right?)

Exactly. If a carbonyl group has two alkyl substituents it's a ketone, if it only has one it's an aldehyde, and if it has one alkyl group and an oxygen it is a carboxylic acid or a derivative thereof. One has to look at each functional group together with its immediate surroundings to be able to predict its behavior.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Rhodium
(Chief Bee)
07-08-04 05:45
No 518109
User Picture 
      NMR Identification and Quantitation of GHB/GBL
(Rated as: good read)
    

Identification and quantitation of gamma-hydroxybutyrate (NaGHB) by nuclear magnetic resonance spectroscopy
Chew SL, Meyers JA
J Forensic Sci, Mar. 2003, Vol. 48, No. 2 (https://www.rhodium.ws/pdf/forensic/ghb-gbl.nmr.analysis.pdf)

Abstract
The most common means of identification of gamma-hydroxybutyrate (NaGHB) involves using Fourier transform infrared spectroscopy (FTIR) or gas chromatography-mass spectrometry (GC-MS) of a suitable derivative. However, these methods may be complicated by possible shifts in chemical equilibrium between gamma-hydroxybutyric acid (GHB), GHB salts and the precursor lactone, gamma-butyrolactone (GBL). This paper addresses the technique of proton and carbon nuclear magnetic resonance spectroscopy (1H and 13C NMR) for the direct and accurate identification of GHB and GBL. The application of 1H NMR for GHB quantitation is also discussed.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Raver71
(Stranger)
07-31-04 00:57
No 522804
      i tried gbl a bunch of times but it doesnt...     

i tried gbl a bunch of times but it doesnt give you that happy mood like ghb does..its more euphoric but without the happyness...
 
 
 
 
    armageddon
(Hive Bee)
07-31-04 02:58
No 522839
User Picture 
      really?!     

Did you know that you can convert GBL to GHB by adding 10% w/w of d.H2O to it, heating to >100°C and then adding an equimolar amount of aequous lye (NaOH, KOH etc.) dropwise?

Besides, I don't understand what you mean when making difference between euphoria and happiness - aren't you happy when u get euphoric??? tongue

(I would rather say that GBL has sedative properties, whereas GHB is euphoric...)

Greetz, A

Pleased to meet you hope you get my name.
But whats puzzlin you is the nature of my game!
 
 
 
 
    ApprenticeCook
(Hive Bee)
07-31-04 05:25
No 522874
      ive seen this question many times.....     

ive seen this question many times..... why do people eat the precursor when the drug is so easily made from it and much much better???

i dont know.... weird....
-AC

Its just my opinion, but no-one listens to me anyway, and rightly so...
 
 
 
 
    raybeez
(Newbee)
08-09-04 15:09
No 524439
      Worked, but with low yields     

Swim finally gave this reaction a try following chromic's writeup on rhodium.ws and had some success but seemingly low yields. Swim ran a 1mol rxn and finished with just under 70g of NaGHB(s).

Swim used ACS grade NaNO2, OTC GABA (that had been tested against a small quantity of ACS grade GABA and was found to have identical solubilities in hot/cold dH2O and EtOH) and OTC muriatic acid.

Reagents where dissolved w/ mag stirring in 300mL dH2O and chilled to below 0°C in an ice-water batch. Acid was added via an addition funnel (was worried a pressure-eq funnel would be needed, but vacuum never seemed to build up) and fumes were vented far away from SWIM using tubing.

Acid was added over the course of two hours.. went very slowly at first, keeping the buildup of yellow-brown gas under control in the rxn flask. Near the end, gas evolution diminshed, and the last 1/3rd of acid was added pretty quickly (over 15-20min). After acid addition, flask sat and stirred and bubbled at 0°C for an hour. At this point, stirring was turned off, and the rxn flask was allowed to sit overnight for 14hrs.

Upon returning, the temp was around 20°C and no bubbling was observed. Swim proceeded to setup flask for simple distillation and began steam distilling off GBL/water, but noticed as the temp increased and stirring was turned back on small gas bubbles formed in the flask (perhaps hadn't finished reacting yet?) Steam distillation continued into NaCl precip. was observed. Distillate was refluxed with ACS NaOH, boiled with 5% activated charcol, filtered, heated to 140-150degC to boil off H2O/excess lactone, and poured into pyrex dish...giving 20g or so of NaGHB. Product was hard, pure white in colour, looked identical to the product of a NaOH/99.9% GBL rxn (yay!). Had a slight tangy aftertaste however (butryic acid maybe?)

Remainder of aqueous was extracted with 5x230mL washes of ethyl acetate. Solvent was removed under vacuum, then swim was planning on distilling off the GBL, but when the temp hit around 50°C in the distillation flask, swim's vacuum failed (one of the joints in the apparatus was the wrong size, and was being held together with parafilm which seemed to melt off ruining the seal).

Distillation was continued until 92°C at 1 atm, then the 48mL of resulting yellowish/brown liquid was reacted with NaOH, boiled with activated carbon, filtered, re-heated to 140-150 °C then poured into a pyrex dish and allowed to harden into NaGHB. Yield was 48g of slightly brownish NaGHB. Swim was worried about product purity, but it tasted and smelled _fine_ (even better then the white NaGHB recovered earlier). Of course was bioassayed and +ve results (no difference in required dosing noted to 0.1 of a gram).

So... 70g yield. swim was expecting close to double that from this reaction.. what went wrong? Rxn not go to completion at the beginning? Solvent washes done incorrectly? Toss some ideas at swim as he is planning on doing the 3mol version of the run soon.
 
 
 
 
    fierceness
(Hive Addict)
08-10-04 20:55
No 524672
      It really sounds like you did everything ...     

It really sounds like you did everything right, even better than when I did it.  The only thing I can see that may have caused it is that you should really not want to see ANY yellow/brown gas because seeing that gas means that there will not be enough nitric acid in solution deaminating the GABA.  If you have a problem controlling the gas, maybe you could add a slight excess of sodium nitrite and HCl.  Other than that, I can't see anything wrong!
 
 
 
 
    Bwiti
08-16-04 01:55
      Lets Fucking Face It..
(Rated as: no sources!)
    
 
 
 
    fierceness
(Hive Addict)
08-17-04 18:33
No 525931
      Pills     

You dont want the kind in pills or even in capsules.  There exists some GABA in powdered form that you're supposed to mix in water or a protein shake or whatever.  This kind of GABA works for this synth.
 
 
 
 
    18294
(Hive Bee)
08-18-04 17:10
No 526092
      SWIM's slight modification     

SWIM may attempt to make some GBL in the near future. Here is a rough outline of his plans:

Using Sandmeyer rxn to turn GABA into GBL (well hopefully, anyway)

1. SWIM will add 1 part powdered Gamma Amino Butyric Acid,  0.68 parts Sodium Nitrite, and he will also add the appropriate amount of water.

2. Next He will titrate his acid

3. He will wait 2 or 3 days for the rxn to complette.

4.He will then add dichloromethane

5. He will titrate his Base (50% NaOH)

6. SWIM will then seperate the water layer and run it through an Activated Charcoal column

7. He will acidify it until it reaches a pH of 6.5

Does anyone have any comments or anything to add to this? SWIM has done quite a bit of reading on the subject, and believes his A/B extraction of the product in combination with an AC clean would be a good substitute for the recomended distillation.
 
 
 
 
    merbst
(Hive Bee)
08-18-04 19:56
No 526100
      Re: believes his A/B extraction of the product     


believes his A/B extraction of the product in combination with an AC clean would be a good substitute for the recomended distillation



As stated in this thread, there is no good substitute for the recommended distillation.  Although of course you are welcome to try! If you have success (or failure even), The Hive is happy to read what you have to say about it!  Beware of the brown gas!  Perform under a fume hood if possible, but don't put your life in the hands of your local electricity provider.

 
 
 
 
    bbeeasheets
(Newbee)
08-28-04 00:42
No 527852
      sodium methoxide     

well after  making about 400g of GBL i took a portion aside to experiment with. One portion I added %50 NaOH (to the dcm extraction) and decanted the aqeouus. At this point I forgot to neutralize with vinegar and just boiled off the water. I took about 40g and and disloved it in boiling meoh (just enuff to disolve it all while stiring). Well the solution gradually became purple! I thought this was weird so I went back over my notes, and saw that I didn't neutralize. So I did some googling and found out that methanol and excess NaOH makes Na-methoxide... but nothing about it going purple. Is this sample salvageable? (without reconverting to gbl and distilling). I hate to toss it.
 
 
 
 
    wimpy
(Hive Bee)
09-29-04 18:25
No 533772
      I'm sorry, but isn't there any alternative to...     

I'm sorry, but isn't there any alternative to sodium nitrite? Sodium Nitrite seems controlled here ... (- after searching a long time now for lots of different chemicals i have to state that the "responsible department" is doing a really good job in barring one's way ... especially annoying as GABA is so easy to obtain mad)
Nothing known? or even thinkable?
thanks

one could start feeling like shooting someone might be at least a little satisfaction :(( ...
 
 
 
 
    Rhodium
(Chief Bee)
09-30-04 03:22
No 533833
User Picture 
      NaNO2 Preparation     

Post 458114 (gruns: "Preparation of Sodium Nitrite: Discussion", Chemicals & Equipment)

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    wimpy
09-30-04 19:24
      Thanks Rhodium, sounds promising!
(Rated as: UTF PM Function)
    
 
 
 
    wimpy
(Hive Bee)
10-03-04 18:59
No 534297
      There's probably no way to separate NaNO2 from     

There's probably no way to separate NaNO2 from NaCL out of a mixture of both (1-0.5% NaNO2 in NaCL)? All swim was able to find out was that both are soluble in H2O but not so good in alcohol ...

- Beware of the Morphail Effect! -
 
 
 
 
    Rhodium
(Chief Bee)
10-03-04 20:34
No 534311
User Picture 
      Solubility of NaNO2 & NaCl at different temps
(Rated as: good read)
    

0009-004-sol-v-t.gif fig9-1.gif

I'd disagree. Check the tables above for a correlation of aqueous solubility of salts at different temperatures. The left shows NaCl and the one on the right shows NaNO2. As anyone can see, the solubility of NaCl does not differ much with temperature (it is always at 35-40g in 100mL water) while the solubility for NaNO2 more than doubles from 75g/100mL at 0°C to 165g/100mL at 100°C.

Thus extract the NaCl/NaNO2 mixture with boiling water (sodium nitrite being over four times more soluble than the chloride), then concentrate the extract to precipitate sodium chloride preferentially and filter hot (at room temp the solubility difference is much less).

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    wimpy
(Hive Bee)
10-04-04 18:32
No 534406
      Hey! Really thanks a lot - that's kind of...     

Hey! Really thanks a lot - that's kind of light at the end of the tunnel :)
But do i get this right? As far as i understand one would not be able to get pure Nitrite out of this, or ... ?
So this leads to the question: would a smaller amount of NaCL affect the reaction?
Anyway, thanks a lot, swim will try as soon as possible!

- Beware of the Morphail Effect! -
 
 
 
 
    Rhodium
(Chief Bee)
10-04-04 20:51
No 534421
User Picture 
      Nitrite enrichment by fractional crystallization     

But do i get this right? As far as i understand one would not be able to get pure Nitrite out of this, or ...?

You have very good prospects for purifying the nitrite - for each iteration of a fractional crystallization procedure using the bare minimum of water needed to dissolve the nitrite (but not more than that as to avoid dissolving too much NaCl) you will remove 75%+ of whatever amount of NaCl you still have left in your salt mixture. If I have calculated it all correctly you will have enriched the nitrite content by three orders of magnitude in five recrystallizations (or less!). If you start out with a NaCl:NaNO2 ratio of 100:1 you will soon have changed that to 1:10...
100:1 → 25:1 → 6:1 → 3:2 → 4:10 → 1:10


The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Agni
(Stranger)
10-25-04 04:14
No 537613
      using a retort     

i really want to try this synth but i dont have a disstilation unit or the money to buy one. Could i use a retort instead of the "normal" flask/condenser method? they are a good deal cheaper.
 
 
 
 
    Rhodium
(Chief Bee)
11-13-04 14:44
No 541379
User Picture 
      GHB & GBL Reactivity in Alcoholic Solutions
(Rated as: excellent)
    

The reactivity of gamma-hydroxybutyric acid (GHB) and gamma-butyrolactone (GBL) in alcoholic solutions
Hennessy SA, Moane SM, McDermott SD,
Journal of Forensic Sciences, Vol. 49(6), 1-10 (2004) (https://www.rhodium.ws/pdf/forensic/ghb.gbl.reactivity.alcoholic.solutions.pdf)

Abstract
In this work the stability of GBL (gamma-butyrolactone) and GHB (gamma-hydroxybutyric acid) in alcoholic media was studied. Under acidic conditions the GBL will react with ethanol or methanol to give the corresponding ethyl and methyl esters of GHB. It can be seen that ester formation is dependent on the type of alcohol, the alcohol content of the solution, and the pH of the solution. Under the same conditions it was shown that GHB does not give rise directly to the corresponding ester when merely in the presence of an alcohol; however the ester will be formed if the conditions are present for conversion of GHB to GBL followed by subsequent reaction with alcohol. In alcoholic beverage samples spiked with GBL the expected conversion to GHB occurred, and the formation of the ethyl ester of GHB was also seen in some samples. Wine samples were analyzed for the presence of the ethyl ester of GHB, and the effect of adding GHB/GBL to hot beverages was studied.

The Hive - Clandestine Chemists Without Borders
 
 

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