The Vespiary

The Hive => Methods Discourse => Topic started by: wacko_reaco on March 21, 2002, 08:19:00 PM

Title: MeAm from hexamine and HBr
Post by: wacko_reaco on March 21, 2002, 08:19:00 PM
Would this work better than with HCl using normal conditions, any thoughts, is MeAM.HBr as deliquessiant as the chloride, is NH4Br soluble in water, i think i should get my CRC out

wacka wacka wacka
Title: HBr
Post by: Rhodium on March 22, 2002, 10:41:00 AM
I believe it would be completele unnecessary to use HBr - as far as I know, the bromide salts are even more hygroscopic/water soluble.
Title: waco
Post by: cheeseboy on March 23, 2002, 04:40:00 PM
Title: I think he's on the right track by trying to ...
Post by: Bwiti on March 26, 2002, 11:41:00 PM
I think he's on the right track by trying to think of a cleaner, less tedious way to make methylamine. Damn, ain't that ammonium cloride a bitch to separate from the goods. If there was an over-priced solvent that would take advantage of their differences, I'd definately buy it! 8)

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Title: MeOH works really well
Post by: Chromic on March 27, 2002, 04:44:00 AM
MeOH works very well to separate MeAmCl from AmCl. It's gives a decently pure MeAmCl, but most important, it's very efficient and easy to use. I've been procrastinating on doing a writeup for the hive... but the method is easy and works well.
Title: No solvent extraction necessary.
Post by: terbium on March 27, 2002, 08:29:00 AM
Damn, ain't that ammonium cloride a bitch to separate from the goods.
I don't find it difficult. If you go through the proper stages of concentrating the aqueous reaction mixture and filtering off crops of ammonium chloride then when the methylamine hydrochloride crystallizes from the reaction mixture it will be sufficiently free of ammonium chloride that it won't need the "extraction with hot anhydrous alcohol" step.
Title: no time
Post by: wacko_reaco on March 28, 2002, 12:37:00 AM
it really would be a breeze, the ammonium bromide is soluble in acetone and ether. The whole mix could simply be roughly dehydrated on the rotovap then immersed in acetone. The only thing i don't know is if the meAm.HBr is also soluble in acetone, the hydrochloride salt is not, anyone know. I think the reaction would proceed better using HBr also. Might do a small trial, couldn't hurt.

wacka wacka wacka
Title: I would expect both to be soluble.
Post by: terbium on March 28, 2002, 07:50:00 AM
Since ammonium bromide is soluble in acetone while ammonium chloride is not then I would expect methylamine.HBr to also be soluble in acetone.
Title: damm
Post by: wacko_reaco on March 29, 2002, 11:58:00 PM