The Vespiary

The Hive => Methods Discourse => Topic started by: ZZACk on November 27, 2001, 04:39:00 PM

Title: hydroxalamine in nabh3cn?
Post by: ZZACk on November 27, 2001, 04:39:00 PM
if one were to  use a dry meoh/ ketone solution and use hydroxylamine instead os annac or methylamine in a slightly acidic solution.before adding nabh3cn.
would one make mdoh or would they have to form the oxime then rereduce it?
hypothetically speaking of course.
Z

Go Ugly Early
Title: Re: hydroxalamine in nabh3cn?
Post by: Rhodium on November 27, 2001, 06:05:00 PM
That would produce MDOH, see

http://www.erowid.org/library/books_online/pihkal/pihkal114.shtml (http://www.erowid.org/library/books_online/pihkal/pihkal114.shtml)



If MDOH is heated too much (as in distillation for example), it disproportionates into MDA and MDP2P oxime.
Title: Re: hydroxalamine in nabh3cn?
Post by: ZZACk on November 28, 2001, 10:57:00 AM
thanks rhod,
would one go about extracting the unreduced ketone, and removing the mdoh in dcm and then gassing or would another solvednt bee better? also how would one remove the meoh without convertingf the mhoh to oxime and mda i would guess with a vaccum distillation.
Z

Go Ugly Early
Title: Re: hydroxalamine in nabh3cn?
Post by: Rhodium on November 28, 2001, 12:30:00 PM
Follow the exact procedure in Pihkal and you'll be fine. There is very little unreduced ketone in there, mostly the ketone reduced to the alcohol.