The Vespiary

The Hive => Methods Discourse => Topic started by: LD_50 on August 09, 2000, 01:01:00 AM

Title: mda with out sodium cyanoborohydride
Post by: LD_50 on August 09, 2000, 01:01:00 AM
anyone with a good referance or scan of a synth for mda without the use of exotic reducing agents or difficult to obtain chemicals? a semisythetic route from i-safrole or 3,4-methylenedioxyphenylacetone would be great...
Title: Re: mda with out sodium cyanoborohydride
Post by: Osmium on August 09, 2000, 02:17:00 AM
Huh?

Look at the thread at the top of this forum. Or search for the Leuckart reaction which uses formamide (from ammonium formate).
Title: Re: mda with out sodium cyanoborohydride
Post by: Outcast on August 09, 2000, 11:35:00 PM
An easy way to make MDA from MDP2P is to first make the oxime by reacting the ketone with hydroxylamine-HCl. This can be done in good yields (>90%). See CA -55, 10595 for details.

The formed oxime is reduced by adding a 10 molar excess of sodium pieces to the oxime in anhydrous EtOH. See J. Chem. Soc. Perkin. Trans 2, -97, pp249-56 for a good procedure. This gave 3.2g MDA from about 4g oxime using 6g sodium and 50ml EtOH. If you're interested I can do a write-up on this...
Title: Re: mda with out sodium cyanoborohydride
Post by: bizwax on August 10, 2000, 12:30:00 AM
You betcha Outcast. We all love new write-ups 'round here. Try to keep in mind a lot of us are just kitchen chemist's. Lookin forward to it  8)
Title: Re: mda with out sodium cyanoborohydride
Post by: Antibody2 on August 10, 2000, 06:44:00 AM
LD 50 - check uot the leukart like Osmium says, antibody did alot investigating in that area a while back and is very OTC as well as simple rxn to do. More variations that you can shake a stick at. Antibody is currently tryying to find some of the MW refs which yield MDA or rather the formyl intermediate in MINUTES!

Outcast is that elemental sodium you refer too? Antibody would love to see a write up on that route. Remember reading some proceedures put forth by Rhodium a while back, they sounded abit more involved than what you are proposing.


Jimi loves ya!
Title: Re: mda with out sodium cyanoborohydride
Post by: LD_50 on August 11, 2000, 12:14:00 PM
yes I did a search of both boards..but could not find any posts that had the rxn. I will check the chemical abstracts this weekend. If somebody has a scan/writeup please post :)
thanks a bunch everyone
Title: Re: mda with out sodium cyanoborohydride
Post by: foxy2 on August 11, 2000, 12:56:00 PM
What will you search CA For
mda with out sodium cyanoborohydride
lol
Title: Re: mda with out sodium cyanoborohydride
Post by: LD_50 on August 11, 2000, 01:01:00 PM
ok..very funny...
Title: Re: mda with out sodium cyanoborohydride
Post by: LD_50 on August 11, 2000, 01:10:00 PM
Foxy2: Tell me how you like this CA search string

"getto AND otc AND mda AND cheap AND easy AND reactor AND no sodium cyanaborohydride"-lol

found it!!! JOC, april '88,p4555,

"the getto reaction for producing mda via OTC chemicals"
by: Sloth T. Helvetrochner phd

Title: Re: mda with out sodium cyanoborohydride
Post by: harry_lime on August 15, 2000, 05:58:00 AM
Whats happend to outcast ?
Thew writup would have been usefull.


I just couldn,t resist asking !
Title: Re: mda with out sodium cyanoborohydride
Post by: Sonson on August 15, 2000, 11:42:00 PM
Heh, this is outcast with my original alias (sonson). I had some problems with my account. And the writeup...almost done...just have to make my dreams more colourful...add more details. Hang on...
Title: Re: mda with out sodium cyanoborohydride
Post by: harry_lime on September 02, 2000, 04:41:00 AM
Still hangin !


I just couldn,t resist asking !
Title: Re: mda with out sodium cyanoborohydride
Post by: frost on September 03, 2000, 11:02:00 AM
were hangin as well outcast, this sounds pretty intresting!
frost
Title: Re: mda with out sodium cyanoborohydride
Post by: tomjuan on November 28, 2001, 07:17:00 AM
This document on Rhodium's site

https://www.thevespiary.org/rhodium/Rhodium/chemistry/mda.dalcason.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/mda.dalcason.html)

seems to imply that MDP2P can converted to MDA in one step, using ammonia and either the amalgam method or the Raney Nickel method. Is this not the case?
Title: Re: mda with out sodium cyanoborohydride
Post by: Rhodium on November 28, 2001, 07:28:00 AM
The amalgam route using ammonia (or ammonium salts) is very low-yielding (20-30%), I don't know about the catalytic hydrogenation with Ni though.
Title: Re: mda with out sodium cyanoborohydride
Post by: zooligan on November 28, 2001, 11:16:00 AM
Raney requires high pressure (supposedly).  There's a link on your (Rhod) page which is a compendium of journal articles.  One is from a Russian Law Enforcement journal detailing how a lab there made MDA using high-pressure CTH.

z

"And if we don't get some cool rules ourselves, pronto, then we'll just be bogus too!"
Title: Re: mda with out sodium cyanoborohydride
Post by: cheeseboy on December 09, 2001, 07:15:00 PM
TETRANITROMETHANE!!!!!  BOOOOOM!!!

May The Source Bee With Yous