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Corrosive Joeseph
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RoundBottoms re-post of "Chromic's Methylamine HCl" always looked very doable as well...............
https://www.thevespiary.org/talk/index.php?PHPSESSID=738fea2...
/CJ
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Melgar
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Quote: Originally posted by PirateDocBrown | 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. |
Even better: if someone needed methylamine for (heaven forbid) a reductive amination, they could do this reaction in one pot, with an excess of
methanol or ethanol, then as soon as the reaction started smelling of methylamine, add the substrate that needed to be aminated. This could work with
other nitro compounds as well, I'd imagine.
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byko3y
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Any1 have idea how to make anhydrous MeNH2 gas in good yield starting from anhydrous MeNH3Cl or some other salt? I didn't expect the task to be so
hard, but that's true: you can't just add NaOH, heat the solution and expect the yield to be high - most of the MeNH2 will be left behind in the NaOH
solution.
Any ideas?
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Melgar
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MeNH2 is very water-soluble, which is the problem. Best advice I can give is to use KOH instead of NaOH. It's a stronger base, and is better at
forcing solutes out of an aqueous solution. Extract with ether or something, then dry, if you need it anhydrous.
KOH is also better at getting an organic layer to form when NaOH can't do it.
I get the feeling that the formaldehyde + NH3 + HCl route is basically a combination of the Cannizzaro reaction and the Leuckart reaction. If you
didn't have much formaldehyde and did have formic acid, the Cannizzaro reaction could perhaps be skipped, even, making for a faster reaction.
Lowering the pH would speed the reaction up too, since it wouldn't depend on the Cannizzaro reaction for formic acid. Assuming my logic is correct,
anyway.
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