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LD5050
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looking for a good proceedure for methylamine
I just found a bunch of hexamine fuel tabs in some old camping equipment I have and I would like to make some methylamine from it. Does anyone know of
where I can find a good write-up ? I have found a few but they seem to contradict each other. Is there a tried and true method floating around
anywhere?
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gluon47
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I've always used the write up on erowid to prepare methylamine (link), just substituting their crude makeshift equipment for proper laboratory glassware.
It's poorly written and layed out, but has always worked just fine for me.
reality is an illusion 
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LD5050
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Yes I saw this one but thought I couldn't trust it because how it was written and the equipment used. If I'm going to make it I would like to at least
have something pretty pure if I'm going to take the time and make it. You said you got good results tho?
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JJay
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Everyone knows that it is impossible to make methylamine. Didn't you watch Breaking Bad? 
I have not personally made methylamine and have no plans to, but there are dozens of procedures on the various drug-making sites on how to do it. I
remember noticing that in the procedures I read, people using procedures involving hexamine paid much less attention to temperature control than
people using more more formal procedures involving formaldehyde and ammonium chloride. I'm pretty sure that this is due to laziness rather than any
good reason and that temperature control is critical for controlling the degree of methylation, but I can't say for sure.
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Tsjerk
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I can confirm temp control is very important, plus a lot of patience to evaporate enough water while you have no clue how far too go. I didn't like
the reaction at all and gave up.
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Melgar
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The trouble with using hexamine is that you also get dimethylamine and trimethylamine, it's slow, and you end up with methylamine hydrochloride in
solution, which isn't necessarily the form that you want. Aluminum/galinstan alloy in nitromethane mixed with a suitable hydrogen donor (water +
methanol, usually) will reduce the nitromethane to methylamine gas pretty easily. You just need to use a suck-back prevention device, and possibly a
desiccant.
edit: for the record, the only reason I've done this so much is to test the reducing power of this aluminum alloy I've been experimenting with, and
both nitromethane and methylamine have very distinctive odors.
[Edited on 3/11/17 by Melgar]
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LD5050
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Since the hexamine method doesn't produce pure methylamine and has many side products could one just maybe drip a NaOH solution into the
methylamine/side product mix and drive off the gas into water and then acidify the water ( I think) to form pure methylamine HCL?
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Melgar
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No. The side products are volatile amines also.
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LD5050
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If I go with the hexamine route I can recrystallize with iso propyl alcohol and wash with chloroform to obtain pretty pure methylamine?
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Tsjerk
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Both formaldehyde and ammonium chloride should be easy to get, I would go that way.
For the heating I would try to make something automated that you don't have to babysit and can not overheat, otherwise, as said, you will need a lot
of patience with the constant danger of burning your reaction mixture.
Maybe that frying pan suggested in the link isn't that bad of an idea, set it to 110 and wait. According to www.sigmaaldrich.com/catalog/product/aldrich/m0505 methylamine hydrochloride doesn't decompose way beyond that, but you don't want to evaporate
your formaldehyde. I would put something aircooled column-like over the outlet, to condense as much formaldehyde back into the pot. https://www.tedpella.com/msds_html/18508msd.htm
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LD5050
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Is there a way to get the formaldehyde out of the campa chem? It says it is a mix of MeOH and formaldehyde but I cant find the percentages I'm having
trouble finding the MSDS on it. It's a liquid and a really dark blue color. I picked it up one day randomly because I remembered reading some people
use to extract the formaldehyde from it but I can find much on it anymore.
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JJay
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I've been meaning to try getting formaldehyde out of Campa Chem but have never gotten around to it.
I think you could evaporate the liquid off at low temperature to produce paraformaldehyde and then heat it to produce formaldehyde gas. There is also
a variety of Campa Chem that consists of paraformaldehyde and some dyes.
Formaldehyde solutions are widely used by non-chemists for things like preserving biological specimens, so they are easy to buy.
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AvBaeyer
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You can easily hydrolyze N-methylformamide with 6M hydrochloric acid to get N-methylamine hydrochloride. Though N-methylformamide may not be cheap,
neither is time and failed touchy preps from hexamine. I have posted somewhere on the site the hydrolysis of N,N-dimethylformamide to obtain
dimethylamine hydrochloride.
Here is one current listing for methylformamide:
http://www.ebay.com/itm/N-Methylformamide-99-7-for-proteomic...
AvB
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cubalibre
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This topic was extensively discussed on this forum.
See https://www.sciencemadness.org/whisper/viewthread.php?tid=12...
It however lacks to discuss the risks involved when mixing formaldehyde and HCl i.e. read: https://www.ncbi.nlm.nih.gov/pubmed/6951075
Maybe hydrolysis should be done using H2SO4 instead of HCl to prevent forming BCME.
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LD5050
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What about making ammonium methylsulfate from sulfamic acid and heating it to high temperature? This makes methylamine but does it also create
dimethylamine? I guess I want to try to make as little dimethyamine as possible seeing as how this is the hardest to remove from the final product.
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Melgar
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If you have hexamine, that's a condensation product between ammonia and formaldehyde, so putting it in hydrochloric acid will hydrolyze it back. You
just need to have enough acid to neutralize the ammonia that's evolved. The acid also catalyzes the Cannizzaro reaction with formaldehyde, if I
remember correctly, and produces formic acid, which is an effective reducing agent for the imine that's being formed.
Formaldehyde can be obtained easily from trioxane, paraformaldehyde, even the plastic polyoxymethylene, just by heating in acid.
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RebekAbrin
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There's a way to synthesize via ammonia chloride reacts with formaldehyde.You could find it on the book SECRETS OF METHAMPHETAMINE MANUFACTURE by
uncle fester,and also you can find this book in PDF on google.
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RebekAbrin
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By the way,the product made by this way is the hydrochloride salt of methylamine,if you wanna make the methylamine gas then add sodium hydroxide
solution to the methylamine hydrochloride.And if you wanna make methylamine solution,thus pass the gas into water with a pipe.
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Tsjerk
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Thank you very much for that elaboration RebekAbrin...
On topic of para-formaldehyde as an intermediate for the purification of formaldehyde:
If you evaporate everything low boiling, which is there to prevent polymerization (methanol), and than freeze and thaw a couple of times you will get
the solid para-formaldehyde. There is no need to make formaldehyde gas from this except if you really need it as a gas, just boiling in water will get
it dissolved again.
You can even use para-formaldehyde a "pure" form of formaldehyde, as it will form free formaldehyde in any heated reaction.
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Texium
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12-3-2017 at 11:09 |
PirateDocBrown
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Just steal some from a passing train.
Seriously, I have made it myself from sulfamic acid, which is cheap and widely available. You will always get some dimethylamine as a side product, no
matter which route you take.
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Melgar
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Not if you reduce nitromethane.
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PirateDocBrown
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That's a good point, but what would you use as a reducing agent?
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Melgar
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Aluminum, activated with a metal or alloy that's liquid at room temperature. Mercury works, of course, but I use a eutectic gallium/indium alloy.
You generally need to add methanol, because it allows mixing with nitromethane, and some water as a hydrogen donor.
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JJay
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PirateDocBrown
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Quote: Originally posted by Melgar  |
Aluminum, activated with a metal or alloy that's liquid at room temperature. Mercury works, of course, but I use a eutectic gallium/indium alloy.
You generally need to add methanol, because it allows mixing with nitromethane, and some water as a hydrogen donor. |
That's very clever!
I've also gone the NH4Cl/CH2O route, in a steam distillation setup, so the water carries over the MeNH2. Of the two, I'd have to say I much prefer the
reforming of sulfamic acid via ammonium methylsulfate.
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