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All 13 posts Subject: Simple Questions Please login to post Down

Schwa
(Stranger)
05-09-04 16:44
No 506015
      Simple Questions

Two things really...For the first refer to the clever ketamine synth posted by antocho that uses totally unwatched materials. One of the last steps requires something called dioxane dibromide. I can imagine what it is, but can't find it in a couple of popular catalogs. What is it for and can something perhaps be substituted for it. It is good work and easy to follow up to that point...
The second concerns dessication of ammonium acetate. I have used the f out of tfse and have not been able to read anything wholly definitive. I suspect that I could do cutting edge reserch to determine an optimal process, but I am an idiot. Usually what I think of has already been done in droves by baby boomers and all their sorry limp dick overly self important asses stand for (Better quit that or get reposted to the couch) or overly industrius jesuitical chemists who have worked out most things to the limits of physics.

Anyway, anyone care to shed a little know how on me either way.

After all, I am just an upside down e.

psyloxy
(Hive Addict)
05-09-04 17:22
No 506021
User Picture       Dioxane + Br2 __> dioxane dibromide The...

Dioxane + Br₂ ^__> dioxane dibromide
The bromides bond lightly to the ethers oxygens giving a more sterically hindered and thus more selective brominating agent.

N-bromo-succinimide would likely be able to substitute, but I guess that's unnecessary.

--psyloxy--

Schwa
(Stranger)
05-09-04 18:52
No 506029
      Okay

Thanks. Stericaly hindered brominating agent...that clears things up. You really feel good that NBS would work as a substitute dioxane dibromide? You would not want to get that close to a smokable yield and fuck things up.

After all, I am just an upside down e.

psyloxy
(Hive Addict)
05-09-04 19:12
No 506034
User Picture       Chemistry gives a rats ass about my feelings.

Chemistry gives a rats ass about my feelings. NBS is a sterically hindered brominating agent, as is dioxane dibromide, that's all I know.

--psyloxy-

Schwa
(Stranger)
05-09-04 19:42
No 506037
      Oh My...So Presumptuous

Thanks for your keen advice. We know how to use a dessicator, but it is the selection and particular preparation of a dessicant that remains in question. Also there are other possible methods that are suggested and it should be reasonable to ask such questions on a board such as this without having to submit to the wreckless scrutiny of a pompous selfimportant know it all looking for someone to give shit to.

After all, I am just an upside down e.

moo
(Hive Bee)
05-09-04 21:52
No 506068
      NBS works because it liberates Br2 when ...

NBS works because it liberates Br₂ when reacting with HBr, which itself is usually liberated when a substrate is brominated by Br₂, thus keeping the concentration of free elemental bromine low in the reaction mixture. This hasn't got much to do with how sterically hindered it is as the brominating species is still Br₂.

I think sodium acetate, which is quite hygroscopic, is usually dried by fusing it, resulting in anhydrous sodium acetate.

_{fear fear hate hate}

ning
(acetaminophanatic)
05-10-04 02:41
No 506122
User Picture       Hrm.

Why does steric hinderance matter?

I was under the impression he was using dioxane bromide because it was easier to handle than liquid bromine. Seem to remember something about this on the hive...here's a preparation of it: Post 255319 (PrimoPyro: "Re: Dioxane dibromide", Chemistry Discourse)
More on it...seems there's no clear statement of its advantages, though: Post 285923 (Antoncho: "Bromoacetone Synthesis", Novel Discourse)
If you're looking to do RESEARCH, read:

My thread: Post 505521 (ning: "Modified ketamine method", Novel Discourse)
A good idea: Post 465673 (Manichi: "Discussion on possible ketamine analogs", Novel Discourse)
A whole lot of links: Post 450682 (AcidPulse: "Ketamine Synthesis", Methods Discourse)

Now, zealot's synthesis is good, but long. If you're looking to innovate, well...I salute you.

Why do you want dry ammonium acetate?
It appears ammonium acetate decomposes much over 114 C. It turns into acetamide, among other things. See https://www.rhodium.ws/chemistry/amide.preparation.html

In fact, dehydration of ammonium acetate by any strong method will yield acetamide. Or is that what you want to make? Methylamine? If so, you should just say that.

BTW, bristling with barbs and shouting "don't tread on me" isn't going to get your questions answered better. Why do people turn so macho when they get on the internet? Just bee nice, and show you're willing to do some work researching, and it will greatly please the people who spend most of their waking hours answering questions of people like you and me. Then you will probably get answers faster and better. If you want to get some respect, do it with knowledge and keen insight. Just a suggestion wink

_{...it's an AOL chatroom for dyslexic spider monkies...}

ning
05-10-04 13:52
      Heh....teasing fun.....
(Rated as: insignificant)

Schwa
(Stranger)
05-12-04 01:09
No 506561
      Freak on...

the dry ammonium acetate is for the nitroethane condensation. Not sure it will improve yields compared to using the hydrate, but it might. May turn out that it not worth the effort; we should certainly be able to buy the dry salt. In reality we became simply curious about how to go about dehydrating the compound. This for sure is not new science. Someone out there has a preference.

We could always go a diferent route to styrene from benzaldehyde, but we like like the classic Shulgin method.

The ideas on the dioxane dibromide/NBS topic are interesting. Moderating the bromine concentration makes sense. You wouldn't want to over brominate.

After all, I am just an upside down e.

ning
(acetaminophanatic)
05-12-04 04:34
No 506584
User Picture       Might want to ask rhodium that one

If you are lucky enough to have a lab, some mates, and a decent supply of nitroethane, you are well ahead in the game. I recommend you learn as much as you can before wasting that precious elixir.

Many amines are used as catalysts. Also, phase-transfer conditions have been used. UTFSE and you will have much much to read. Perhaps one of the experienced alchemists here would have a suggestion for good condensing agent from personal experience.

_{...it's an AOL chatroom for dyslexic spider monkies...}

Rhodium
(Chief Bee)
05-12-04 13:09
No 506649
User Picture       drying ammonium acetate

Ammonium acetate is dried by placing it in a desiccator over any desiccant which has a greater affinity for water than it has itself. Examples include KOH, conc. H₂SO₄, P₂O₅ and others

^{The Hive - Clandestine Chemists Without Borders}

Schwa
(Stranger)
05-12-04 23:09
No 506736
      KOH...That's the ticket

We'll try it, Rhodium, and promise to work on our spelling. We bookmarked your link to the commonly misspelled words in response to someone misspelling of the name of the South African gold piece a couple years ago. (not going to try it now) So we know it is important to you.

We are academically familiar with alternative condensation methods. Would anyone care to weigh out an opinion on the favored alternative to the GAA/ammonium acetate styrene preparation.

The alternate K synth looks better than Zealot's, but correct us if we're wrong...aren't the reaents under the radar at step three.

After all, I am just an upside down e.

ning
(acetaminophanatic)
05-13-04 03:33
No 506769
User Picture       Under the radar?

I guess it depends whose radar you're talking about.

The advantage of Zealot's synth is, of course, that it's been done before. If that's all that matters and you can get the materials, go for it. Research is not the goal of all.

I think making cyclopentanone shouldn't bee too much trouble. It's easy, and even if you could buy it, it would probably be cheaper to make. Adipic acid is a nylon industrial precursor, and as such is extremely dirt cheap. I'm not so sure such economies of scale apply to cyclopentanone. Plus it could bee watched. I wouldn't buy it.

Benzyl chloride is useful to make amphetamines. Buy benzyl alchol or something instead. Better yet, as the o-fluoro analog of ketamine is reported to be very nice, buy o-fluorobenzyl alcohol or benzyl chloride. That surely is not a watched chem.

For me, it's just an art form to design all-OTC synthesis. Just because it could be done. Take what you like and drop what you don't. cool

_{...it's an AOL chatroom for dyslexic spider monkies...}

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	All 13 posts		Subject: Simple Questions		Please login to post		Down


		Schwa (Stranger) 05-09-04 16:44 No 506015				Simple Questions
						Two things really...For the first refer to the clever ketamine synth posted by antocho that uses totally unwatched materials. One of the last steps requires something called dioxane dibromide. I can imagine what it is, but can't find it in a couple of popular catalogs. What is it for and can something perhaps be substituted for it. It is good work and easy to follow up to that point... The second concerns dessication of ammonium acetate. I have used the f out of tfse and have not been able to read anything wholly definitive. I suspect that I could do cutting edge reserch to determine an optimal process, but I am an idiot. Usually what I think of has already been done in droves by baby boomers and all their sorry limp dick overly self important asses stand for (Better quit that or get reposted to the couch) or overly industrius jesuitical chemists who have worked out most things to the limits of physics. Anyway, anyone care to shed a little know how on me either way. After all, I am just an upside down e.



		psyloxy (Hive Addict) 05-09-04 17:22 No 506021				Dioxane + Br2 __> dioxane dibromide The...
						Dioxane + Br₂ ^__> dioxane dibromide The bromides bond lightly to the ethers oxygens giving a more sterically hindered and thus more selective brominating agent. N-bromo-succinimide would likely be able to substitute, but I guess that's unnecessary. --psyloxy--



		Schwa (Stranger) 05-09-04 18:52 No 506029				Okay
						Thanks. Stericaly hindered brominating agent...that clears things up. You really feel good that NBS would work as a substitute dioxane dibromide? You would not want to get that close to a smokable yield and fuck things up. After all, I am just an upside down e.



		psyloxy (Hive Addict) 05-09-04 19:12 No 506034				Chemistry gives a rats ass about my feelings.
						Chemistry gives a rats ass about my feelings. NBS is a sterically hindered brominating agent, as is dioxane dibromide, that's all I know. --psyloxy-



		Schwa (Stranger) 05-09-04 19:42 No 506037				Oh My...So Presumptuous
						Thanks for your keen advice. We know how to use a dessicator, but it is the selection and particular preparation of a dessicant that remains in question. Also there are other possible methods that are suggested and it should be reasonable to ask such questions on a board such as this without having to submit to the wreckless scrutiny of a pompous selfimportant know it all looking for someone to give shit to. After all, I am just an upside down e.



		moo (Hive Bee) 05-09-04 21:52 No 506068				NBS works because it liberates Br2 when ...
						NBS works because it liberates Br₂ when reacting with HBr, which itself is usually liberated when a substrate is brominated by Br₂, thus keeping the concentration of free elemental bromine low in the reaction mixture. This hasn't got much to do with how sterically hindered it is as the brominating species is still Br₂. I think sodium acetate, which is quite hygroscopic, is usually dried by fusing it, resulting in anhydrous sodium acetate. _{fear fear hate hate}



		ning (acetaminophanatic) 05-10-04 02:41 No 506122				Hrm.
						Why does steric hinderance matter? I was under the impression he was using dioxane bromide because it was easier to handle than liquid bromine. Seem to remember something about this on the hive...here's a preparation of it: Post 255319 (PrimoPyro: "Re: Dioxane dibromide", Chemistry Discourse) More on it...seems there's no clear statement of its advantages, though: Post 285923 (Antoncho: "Bromoacetone Synthesis", Novel Discourse) If you're looking to do RESEARCH, read: My thread: Post 505521 (ning: "Modified ketamine method", Novel Discourse) A good idea: Post 465673 (Manichi: "Discussion on possible ketamine analogs", Novel Discourse) A whole lot of links: Post 450682 (AcidPulse: "Ketamine Synthesis", Methods Discourse) Now, zealot's synthesis is good, but long. If you're looking to innovate, well...I salute you. Why do you want dry ammonium acetate? It appears ammonium acetate decomposes much over 114 C. It turns into acetamide, among other things. See https://www.rhodium.ws/chemistry/amide.preparation.html In fact, dehydration of ammonium acetate by any strong method will yield acetamide. Or is that what you want to make? Methylamine? If so, you should just say that. BTW, bristling with barbs and shouting "don't tread on me" isn't going to get your questions answered better. Why do people turn so macho when they get on the internet? Just bee nice, and show you're willing to do some work researching, and it will greatly please the people who spend most of their waking hours answering questions of people like you and me. Then you will probably get answers faster and better. If you want to get some respect, do it with knowledge and keen insight. Just a suggestion _{...it's an AOL chatroom for dyslexic spider monkies...}



		ning 05-10-04 13:52				Heh....teasing fun..... (Rated as: insignificant)



		Schwa (Stranger) 05-12-04 01:09 No 506561				Freak on...
						the dry ammonium acetate is for the nitroethane condensation. Not sure it will improve yields compared to using the hydrate, but it might. May turn out that it not worth the effort; we should certainly be able to buy the dry salt. In reality we became simply curious about how to go about dehydrating the compound. This for sure is not new science. Someone out there has a preference. We could always go a diferent route to styrene from benzaldehyde, but we like like the classic Shulgin method. The ideas on the dioxane dibromide/NBS topic are interesting. Moderating the bromine concentration makes sense. You wouldn't want to over brominate. After all, I am just an upside down e.



		ning (acetaminophanatic) 05-12-04 04:34 No 506584				Might want to ask rhodium that one
						If you are lucky enough to have a lab, some mates, and a decent supply of nitroethane, you are well ahead in the game. I recommend you learn as much as you can before wasting that precious elixir. Many amines are used as catalysts. Also, phase-transfer conditions have been used. UTFSE and you will have much much to read. Perhaps one of the experienced alchemists here would have a suggestion for good condensing agent from personal experience. _{...it's an AOL chatroom for dyslexic spider monkies...}



		Rhodium (Chief Bee) 05-12-04 13:09 No 506649				drying ammonium acetate
						Ammonium acetate is dried by placing it in a desiccator over any desiccant which has a greater affinity for water than it has itself. Examples include KOH, conc. H₂SO₄, P₂O₅ and others ^{The Hive - Clandestine Chemists Without Borders}



		Schwa (Stranger) 05-12-04 23:09 No 506736				KOH...That's the ticket
						We'll try it, Rhodium, and promise to work on our spelling. We bookmarked your link to the commonly misspelled words in response to someone misspelling of the name of the South African gold piece a couple years ago. (not going to try it now) So we know it is important to you. We are academically familiar with alternative condensation methods. Would anyone care to weigh out an opinion on the favored alternative to the GAA/ammonium acetate styrene preparation. The alternate K synth looks better than Zealot's, but correct us if we're wrong...aren't the reaents under the radar at step three. After all, I am just an upside down e.



		ning (acetaminophanatic) 05-13-04 03:33 No 506769				Under the radar?
						I guess it depends whose radar you're talking about. The advantage of Zealot's synth is, of course, that it's been done before. If that's all that matters and you can get the materials, go for it. Research is not the goal of all. I think making cyclopentanone shouldn't bee too much trouble. It's easy, and even if you could buy it, it would probably be cheaper to make. Adipic acid is a nylon industrial precursor, and as such is extremely dirt cheap. I'm not so sure such economies of scale apply to cyclopentanone. Plus it could bee watched. I wouldn't buy it. Benzyl chloride is useful to make amphetamines. Buy benzyl alchol or something instead. Better yet, as the o-fluoro analog of ketamine is reported to be very nice, buy o-fluorobenzyl alcohol or benzyl chloride. That surely is not a watched chem. For me, it's just an art form to design all-OTC synthesis. Just because it could be done. Take what you like and drop what you don't. _{...it's an AOL chatroom for dyslexic spider monkies...}

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