00Buckshot
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Methylamine question
Hello everybody.
I was surfing Rhodiums site and I found a meth synth that seems easy for me. Over the past 2 years or so my chemistry learning curve has moved well
IMO. However I'm not that sure about this because the directions for the synth are a touch advanced for me.... Along with most of Rhodiums stuff.
So I thought I'd check it with the two best chemists I know online....And anyone else who can contribute.
This link has several similar methods, but I am refering to the method that uses Hcl with Hexamine to produce the methylamine. Is it that easy? The
writeup doesn't even need any distilling or condensing or any other of that fancy stuff.
http://www.rhodium.ws/chemistry/methylamine.html
Now I realize that maybe I should ask this at the Hive, but the truth is when I read posts at the Hive I end up more confused than I was before, I
know that you guys can explain. Should I stick with even more attempts at match book RP I2 reductions that never work or start trying this Hexamine
method?
Thank you, and I hope someone soon has good results over on that phosphorus synth.
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00Buckshot
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Heres that link again
Messed the link up the 1st time here it is again.
http://www.rhodium.ws/chemistry/methylamine.html
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00Buckshot
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.
I just wanted to clarify that I am refering to methylamine hcl, not to be confused with methamphetamines themselves.
For some reason I can't edit my posts. Maybe I wouldn't need to edit them if would lay of the ganj...hehe.
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madscientist
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This synthesis sounds feasible:
[QUOTE]
Methylamine Hydrochloride from HMTA, Eleusis' version [with comments by Rhodium]
140g of Hexamine is carefully dissolved in 400mL of Muriatic Acid (31.45% HCl) to which at least 100mL of (preferably) absolute ethanol has been
added. Add the hexamine slowly while stirring vigorously and with good ventilation as some nasty fumes are produced. Allow all to stir at room
temperature for at least 8 hours but preferably 16. The solution will become turbid within several hours of the initial mixing. I *believe* this is
the formation of a formaldehyde trimer of some sort and I suspect that the original equation for the conversion of hexamine into methylamine fragments
is therefore incorrect. [There is no trimer of any sort formed, if enough water and formaldehyde is present. Eleusis uses 4 moles of amine to 6
methylenes, which is enough, but gives less yield.] At any rate, filter off this white precipitate which is obviously not an amine salt due to it
being fluffy even in Florida's humidity (almost all simple amine salts are hygroscopic) [With the exception of ammonium chloride, and this is it].
Finally, remove the excess water, hydrochloric acid and freako volatile products by, ideally, heating the liquid at low to medium heat in a porcelain
saucepan. Stove-proof glass would be ideal, but stainless-steel, aluminum and copper are definitely not! [Rather use a RB flask, with a water
aspirator attached, smells considerably less]. The concentration can generally be left unattended for a couple of hours, but try to stick around and
babysit it at least the first time so you will have a good idea of how long it takes for your particular stove/pots/etc... [Or else it'll BURN!] Also,
the methylamine HCl will form a melt if heated too long at which point it will sublimate off. It will then appear as if it's taking forever for the
stuff to concentrate when in fact you are merely boiling your product away. After the concentrated slush has become sufficiently "thick", take it off
the heat every so often to see if it doesn't soldify, insuring that the water is mostly gone and that not too much sublimation has occured (some is
inevitable and even desireable). The yield of Methylamine HCl should be around 200g as white deliquescent crystals. Note, ACS-grade methylamine HCl is
colorless. We aren't using ACS-grade production techniques here, so don't expect ACS-grade product. However, the methylamine produced by this method
is eminently suitable for the many purposes normally intended and if allowed to sublimate some when heating, no adjustment for "purity" or "water
content" need be made in subsequent uses of it. [I can't understand how he can get 200g of product. 140g hexamine gives 80 grams of NH4Cl, and
HOPEFULLY more than 100g of methylamine]. If the crystals are opaque white and do not deliquesce quickly in air of average humidity (65% rh), they may
be contaminated with some Hexamine or some bizarre polymer. [Or ammonium chloride. Recrystallize from methanol, then wash with CHCl3]. Washing 100g of
the crude product with 100mL of Chloroform by stirring in a beaker then filtering, repeated as many times as necessary, will remove Hexamine.
Methylamine HCl is insoluble in Chloroform whereas Hexamine is at the rate of 1g to 10mL. As a final note, I have been informed that hexamine is
available in some areas in the form of "fuel tablets" for small camping stoves. I have received mixed results from various individuals using this so,
as the saying goes, Caveat Emptor.
[/QUOTE]
I weep at the sight of flaming acetic anhydride.
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chemrox
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You can fast forward this a bit by using formaldehyde solution and NH4Cl. Both are readily available most places and not expensive.
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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UnintentionalChaos
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This may well be the most impressive thread necro I've seen in a long time, and what lovely content it has too. Almost 7 years delay for 2 sentences
in a cook thread.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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497
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^Agreed. There should be some kind of award or trophy..
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Nicodem
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Thread Closed
10-4-2009 at 00:39 |
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