The Vespiary

The Hive => Methods Discourse => Topic started by: ZZACk on November 23, 2001, 03:04:00 PM

Title: rextalizing mda
Post by: ZZACk on November 23, 2001, 03:04:00 PM
I've tried this many times with ipa/acetone or ethyl ether. it dosen't dissolve in ipa well or much better in meoh. i haven't tried acetonitrile yet but its on the to do list. best ever distilled freebase mixed with acetone 1:7 then gassed after cooling. also tried neoutralizing with ipa wgassed with ipa and allowed to sit in freezer for larger xtals.
any hints here?
R
Go Ugly Early
Title: Re: rextalizing mda
Post by: sunlight on November 23, 2001, 06:20:00 PM
Yes, IPA is not the option for MDA, methanol would be better.
Neutralizing with IPA gassed and then acetone seems a very good way.
Title: Re: rextalizing mda
Post by: Acme on November 24, 2001, 03:03:00 AM
Maybee make the sulfate instead
Title: Re: rextalizing mda
Post by: AMINATOR on November 24, 2001, 07:37:00 AM
dissolve freebase in ether then add isopropynol that has been mixed with sulphuric acid, till neutral :)
Title: Re: rextalizing mda
Post by: ZZACk on November 25, 2001, 11:14:00 AM
swim used to make the sulphate with sulfurc 20% in ipa, added to dcm, but diden't get big xtals.
it seems the freebase in acetone thing worked for him the best for big white chunks, want to try the acetonitrile thing though for single solvent xtalization. ipa gassed whtn ipa plus diititional ips and let sit in freezer worked also well.
z
Go Ugly Early