ZZACk (Newbee)
11-23-01 15:04
No 239683
      rextalizing mda  Bookmark   

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
 
 
 
 
    sunlight
(Pioneer Researcher)
11-23-01 18:20
No 239702
      Re: rextalizing mda  Bookmark   

Yes, IPA is not the option for MDA, methanol would be better.
Neutralizing with IPA gassed and then acetone seems a very good way.
 
 
 
 
    Acme
(Hive Bee)
11-24-01 03:03
No 239830
      Re: rextalizing mda  Bookmark   

Maybee make the sulfate instead
 
 
 
 
    AMINATOR
(Hive Bee)
11-24-01 07:37
No 239918
      Re: rextalizing mda  Bookmark   

dissolve freebase in ether then add isopropynol that has been mixed with sulphuric acid, till neutralsmile
 
 
 
 
    ZZACk
(Newbee)
11-25-01 11:14
No 240283
      Re: rextalizing mda  Bookmark   

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