The Vespiary

The Hive => Methods Discourse => Topic started by: WW4000 on September 21, 2002, 12:18:00 PM

Title: Damned clear globules ! (
Post by: WW4000 on September 21, 2002, 12:18:00 PM: Why oh Why (I hope this is in the correct zone)

First there were weird looking crystals of Methylamine HCl, next moment all that sits there is a group of clear liquid globules - which themselves will not freeze!

What a damn waste of effort that was, what went wrong?

30%Formaldehyde w/w & 25% Ammonia w/w = Hexamine

Hexamine & 33% HCl w/w = Ammonium Chloride & Formaldehyde ?(yeah- as per Rhodiums page "chemhack")

HEAT with Ammonium Chloride & Formaldehyde = `among other things` Methylamine HCl

After doing the hot alcohol / icy cold alcohol purification process a few times SWIM thought she'd cracked it, and then this! globules ....useless globules man!
I AM A UK BEE, FEEL FREE TO COMMUNICATE REGARDING SPECIFIC UK MATTERS
Title: Vogel
Post by: terbium on September 21, 2002, 02:42:00 PM: If you want to produce methylamine than you should try to follow the procedure from Vogel as closely as possible.
Post 209576 (missing)
(terbium: "Re: Methylamine; So many problems? Is it the Altitude", Newbee Forum)
Title: Methylamine
Post by: Chromic on September 21, 2002, 06:18:00 PM: Remember what Eleusis said? To get this stuff dry before recrystallizing, you gotta heat it until the fumes start coming off. (sublimination of AmCl) Then recrystallize with MeOH, wash with acetone and go from there. If it's very humid, your crystals can turn out wet.
Title: Vogel
Post by: terbium on September 21, 2002, 11:25:00 PM: Remember what Eleusis said? To get this stuff dry before recrystallizing, you gotta heat it until the fumes start coming off. (sublimination of AmCl)
Better to follow the Vogel procedure.
Title: Damn!
Post by: SPISSHAK on September 23, 2002, 07:40:00 AM: I read that link and I thinks your a real pro! ;)