Main Index   Search   Register   Login   Who's Online   FAQ   Links
  2 Online, 0 Active   You are not logged in  
Main Index     The HIVE light edition (TM)
This is a historical archive
The forum is read-only. Private information has been removed. It is not possible to login.


Newbee Forum  

All 15 posts   Subject: Using can tabs as Aluminum in MDMA rxn   Please login to post   Down

 
    MakoEyes
(Stranger)
10-31-04 09:58
No 538898
      Using can tabs as Aluminum in MDMA rxn     

SWIM wants to know if its possible to use the tabs used to open soda cans for the aluminum in a Dr. Drool style MDMA synth. SWIM is fucking addicted to goddamned Mt. Dew and has millions of the little fuckers... this will keep SWIM from fuckign up his/her scissors and save time by not having to cut/prosess all that Rennolds Wrap. The aluminum is some what heavier than that of heavy duty foil so SWIM doesnt think that SWIM needs to make it into any sort of ball but SWIM is however worried that it is to thick and/or contains Tin or something other than aluminum. thanks alot.

"thoes were... Makoeyes!"
 
 
 
 
    ApprenticeCook
(Hive Addict)
10-31-04 11:44
No 538905
      i thought cans were tin with a layer of ...     

i thought cans were tin with a layer of aluminium to prevent corrosion....

So i doubt they can be used, i know cuttin of alu is a pain but its the tried and true way, makes for interesting work while watchin tv i found....

-AC

Its just my opinion, but no-one listens to me anyway, and rightly so...
 
 
 
 
    MargaretThatcher
(Hive Bee)
10-31-04 12:16
No 538906
User Picture 
      Drink Cans     

Are pure aluminium with a thin coating inside.

Are you, or have you ever been a Liberal? YES / NO
 
 
 
 
    hypo
(Balanced Ego)
10-31-04 14:50
No 538912
      actually...     

...it depends on the country. (really!)

HΨ=EΨ
 
 
 
 
    jboogie
10-31-04 18:51
      aluminium flake/powder
(Rated as: hazardous)
    
 
 
 
    Rhodium
(Chief Bee)
10-31-04 20:00
No 538951
User Picture 
      Aluminum flakes are WAY too reactive for Al/Hg     

Aluminum flakes are WAY too reactive for Al/Hg procedures - an explosion is sure to result!

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    psychokitty
(«»)
11-01-04 01:49
No 539006
      Thin or heavy duty foil is all that works . . .     

For the reaction that is the focus of this thread, you should know that experimentation has determined that alternative aluminum products, such as aluminum pie pans, aluminum sheeting, aluminum anything except aluminum foil, do not work as they seem to have other metals within their matrix that hinder the reductive amination. 

Solvents like ethanol or IPA at reflux temperature do not work either (or rather, do not work very well), only methanol and/or other alcohol mixtures.  Methanol can not be from an industrial source as it will likely be polluted with hydrocarbons contaminants that wil create problems during the reductive amination. 

So if you insist on ignoring the already established experimental proceedure, then I suppose you also don't mind wasting your time, money, and likely scarce resources.

For this reaction, it might be advantageous to use cassia oil, a.k.a., cinnamaldehyde, in this reaction just for a low-cost practice run.  I'm pretty sure cinnamaldehyde would react well in the reductive amination as it has a reactive carbonyl group that will form an imine, which can then be reduced to an amine that will likely crystallize in a similar manner to the main product of the standard MM Al/Hg proceedure.
 
 
 
 
    abolt
(Comandante A)
11-01-04 02:17
No 539012
User Picture 
      ?     

Swim has seen Aluminium foil and "Industrial source" Methanol utilised successfully in a Al/Hg.

Swim HIGHLY RECOMMENDS utilising Thick Al in aminations.

To answer your question, "SWIM wants to know if its possible to use the tabs used to open soda cans for the aluminum in a Dr. Drool style MDMA synth", swim would advise you to contact the manufacturer of the cans and enquire as to the make up of the metal. If It's just uncoated Al, then go ahead and use it.

A phone call is all it costs.

http://www.terrorready.net/index.asp
 
 
 
 
    psychokitty
(«»)
11-02-04 02:29
No 539149
      I beg to differ     


Swim has seen Aluminium foil and "Industrial source" Methanol utilised successfully in a Al/Hg.




Even so, as a general rule, "Industrial source" methanol can only be used if it doesn't have any adulterants or contaminants like the hydrocarbons that I mentioned.  Unless the methanol is clearly indicated to be of sufficient purity, use of it is highly ill-advised.
 


Swim HIGHLY RECOMMENDS utilising Thick Al in aminations.




From what source?  If the aluminum is pure, I see no reason why it can't be used.  But the aforementioned aluminum sources have too often provided unwieldy results.  Perhaps using nitromethane -- as opposed to methylamine -- has something to do with this.  I really don't know.  But as far as being consistent, aluminum foil is the only product worthy of recommendation.

 
 
 
 
    Xaja
(Hive Bee)
11-02-04 03:19
No 539157
User Picture 
      Distillation?     

Would distilling the methanol (twice maybe?) be a good idea then?

What? The Land of the Free? Whoever taught you that is your enemy! - Rage Against The Machine
 
 
 
 
    bbeeasheets
(Hive Bee)
11-02-04 04:38
No 539167
      al foil and methanol     

first of all, if you use a paper cutter (the cheap plastic ones  work great from office max), rip off a huge sheet and fold it lengthwise about 4 times before you run it through the cutter, then cut it in about 1 inch strips, throw the hole pile (i cut about 150-200g at a time) in a blender, it only takes about 10-15 minutes. anyways thats what i do. and as for methanol, i distill heet, and thow away first 50 mls and make sure i leave 1/3 volume in the flask. it works perfect for 85% yields in al/hg (round bottom style) based on ketone weight used.

oh before someone throws me off and bans my account or something, is using the name "heet" naming sources?
 
 
 
 
    ApprenticeCook
(Hive Addict)
11-02-04 06:20
No 539180
      its a brand name isnt it?     

its a brand name isnt it? a SOURCE of material for diversion? so yes.

85% yields in al/hg (round bottom style) based on ketone weight used.
Ok, what did you do? weight --> weight yield or molar yields? TOTALLY different.

-AC

Its just my opinion, but no-one listens to me anyway, and rightly so...
 
 
 
 
    bbeeasheets
(Hive Bee)
11-02-04 07:37
No 539185
      sorry about the source then     

sorry about naming source then.

it was weight weight, not molar yield, but thats with distilling freebase and re-xtal from ipa... so i am happy with 85% w/w. if industrial meoh is not used, can better yields be expected?
 
 
 
 
    abolt
(Comandante A)
11-03-04 03:26
No 539332
User Picture 
      Hardware store flashing (Thick Al) & Nitromethane
(Rated as: excellent)
    

From what source?

Hardware store flashing.


Thick Al & Nitromethane

Swim believes this is the easiest and more importantly, the safest way, for the supernewbee to do an Al/Hg nitromethane amination.

If the instructions are followed closely, Supernewbees can do successful aminations, the first time, thereby limiting the waste of valuable and rare precursors. This procedure also allows the chemist to do much larger aminations utilising smaller glassware and using less alcohol, extraction solvents, Hg salts etc. as compared to the thin aluminium aminations [1], thereby allowing further savings on costs and environmental impact.

What makes this process more user friendly is the use of thick aluminium a.k.a aluminium flashing.



The thicker Aluminium paces the reaction much more slowly and allows for a less exothermic reaction. Also, it will allow a much greater methylamine to Ketone ratio, thereby favouring greater product formation.  

Aluminium flashing is found in hardware stores and is used extensively in house building, particularly wooden houses and log cabins.

The aluminium Swim prefers is 0.3 mm or (300 microns) thick and is cut into roughly 1 cm x 1 cm pieces.



The only difference in equipment between this reaction and the Methyl Man reaction is the use of an overhead stirrer. An overhead stirrer is a MUST in regards to this particular technique. An overhead stirrer can be easily made from old electrical parts, for example, a low geared drill press or in this instance, an old electric motor, with a side gear that was salvaged from a garage sale.  



A stainless steel shaft of a suitable length is easily acquired from a hardware/metal working store, and has a blob of weld on the bottom that was filed back to allow a Teflon paddle, cut from a sheet of Teflon to be fixed at one end, whilst the other end can be ground to fit snugly into a detachable chuck, which should be available at any hardware store. [2]



The Reaction

1. A 3 litre Saucepan, containing cool water, is placed upon the hotplate/stirrer.

2. A 3 litre 3 neck R.B.F. is placed in the saucepan and fixed firmly in place so as it doesn’t touch the sides or base of the pan, and is at least half immersed in the cool water.

3. 100 grams of Aluminium is placed inside the 3 lt 3 neck R.B.F. along with 800 mls of MeOH.

4. An overhead stirrer is fixed into the centre neck, with the paddle clearing the sides and base of the R.B.F. and tested to ensure that minimal “wobble” is encountered in the setup.

5. TA condenser is now attached and fixed in place, the hoses attached and connected to the water pump and 20 lt reservoir containing cold tap water & Ice.[7]

6. Now a spatula containing 200- 300 mg of HgCl2 is carefully (gloves) placed through the remaining open neck, via a funnel and the spatula and funnel are rinsed with 80 mls DH2O and 700 mls MeOH, to help wash down any residual HgCl2.

7. A Dropping Funnel is now fixed in the remaining open neck in order to seal the reaction up, the condenser pump and stirrer is turned on and the reaction is left for 30 – 45 minutes to allow for amalgamation to take place. [8]

8. When amalgamation has commenced, load 100 grams of MeNO2 into the Dropping Funnel and commence dripping at a slow enough rate to avoid excess exothermia. [9]




9. After all the MeNO2 has been added, turn on the hotplate and raise the temperature until a slight reflux is noted at the condenser (~ 65 Celsius).

10. When the reflux is observed, pour 100 grams MDP2P along with the remaining 100 ml MeOH into the Dropping Funnel and commence a slow drip of the ketone. [10]



11. When the ketone drip has finished, close the tap on the dropping funnel and allow the reaction to stir and reflux for a further 4-6 hours.

12. When the 4-6 hour period is up, turnoff the heat and allow the reaction to stir overnight.[11]

Next morning Basify, extract, A/B, Distil freebase and gas as usual.

Usual returns are 80-90% w/w ketone to amine salt.

[1] By comparison the Methyl Man technique would require lots more chemicals. Do the math.    

[2] Discussions in the past pertaining to the practicality of the use of stainless steel in a mercurous amalgam have been inconclusive. Swim can state that discoloration of the S/S stirring rod has been the only anomaly noted, and that the reaction proceeds as usual.

[3] Size up or down to suit.

[4] No need for super, turbo charged, nitrogen cooled, condensing. Due to the stability of this reaction, a plain old Leibig condenser is more than sufficient.

[5]  A dropping funnel is not necessarily required, if you have trouble finding one. Once when Swims Dropping Funnel broke, Swim used a plain old glass eye dropper to squirt the Nitromethane (5 ml/3-4 mins) and MDP2P (1 ml/2-3 mins)  down the condenser with normal results (rinse the condenser with a little MeOH, intermittently).

[6] Made via Labtops Performic.

[7] A couple of 2 litre plastic Juice bottle filled with water and frozen does the job nicely. In warmer weather you will need to change over the ice bottles, so have 2 more on standby.

[8] Due to the pace of this reaction we can take much more time with our steps.

[9]  Swim usually takes around 75 – 90 minutes to complete the drip. Once again, with this reaction there is no hurry.

[10] Try to do this as slowly as possible, in order to have a constant excess of Methylamine. 4 - 6 hours is no problem, with 0.3 mm flashing.

[11] Try to occasionally check the reaction, although it should be well under control by now.

http://www.terrorready.net/index.asp
 
 
 
 
    hypo
(Balanced Ego)
11-03-04 11:44
No 539412
      you bastard!     

i wanna have that overhead stirrer too! tongue

imho the only critical thing when doing an Al/Hg is the stirring.

HΨ=EΨ
 
 

All 15 posts   End of thread   Top
   

 https://the-hive.archive.erowid.org    the-hive@erowid.org
   
Powered by Semiconductors v.6.2, 2021, Chemhacks of Honey

Links     Erowid     Rhodium

PIHKAL     TIHKAL     Total Synthesis II

Date: 05-15-24, Release: 1.6 (10-04-15), Links: static, unique