Author Topic: Simple Questions  (Read 2247 times)

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Schwa

  • Guest
Simple Questions
« on: May 09, 2004, 06:44:00 PM »
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.


psyloxy

  • Guest
Dioxane + Br2 __> dioxane dibromide The...
« Reply #1 on: May 09, 2004, 07:22:00 PM »
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

  • Guest
Okay
« Reply #2 on: May 09, 2004, 08:52:00 PM »
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.


psyloxy

  • Guest
Chemistry gives a rats ass about my feelings.
« Reply #3 on: May 09, 2004, 09:12:00 PM »
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

  • Guest
Oh My...So Presumptuous
« Reply #4 on: May 09, 2004, 09:42:00 PM »
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.


moo

  • Guest
NBS works because it liberates Br2 when ...
« Reply #5 on: May 09, 2004, 11:52:00 PM »
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.


ning

  • Guest
Hrm.
« Reply #6 on: May 10, 2004, 04:41:00 AM »
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.thevespiary.org/rhodium/Rhodium/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 ;)


ning

  • Guest
Heh....teasing fun.....
« Reply #7 on: May 10, 2004, 03:52:00 PM »

Schwa

  • Guest
Freak on...
« Reply #8 on: May 12, 2004, 03:09:00 AM »
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.


ning

  • Guest
Might want to ask rhodium that one
« Reply #9 on: May 12, 2004, 06:34:00 AM »
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.


Rhodium

  • Guest
drying ammonium acetate
« Reply #10 on: May 12, 2004, 03:09:00 PM »
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


Schwa

  • Guest
KOH...That's the ticket
« Reply #11 on: May 13, 2004, 01:09:00 AM »
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.


ning

  • Guest
Under the radar?
« Reply #12 on: May 13, 2004, 05:33:00 AM »
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.  8)