dormouse
(Member) 04-25-00 01:14 No 108850 |
Validation of Delepine and of Halosafrole -egotrip | Bookmark | ||||||
the Hive BB Novel Discourse Validation of Delepine and of Halosafrole profile | register | preferences | faq | search next newest topic | next oldest topic Author Topic: Validation of Delepine and of Halosafrole egotrip NewBee posted 02-04-2000 11:38 PM ---------------------------------------- This is the result of much effort ,and the information is as accurate as I can remember. I am sure the colors are correct, and that the times, amounts, etc, are reasonably accurate, I didn't have true scales. The amounts: 1) 25 g dillapiole The dmso was frozen,solid. Removed from icebox. Chilled H2SO4 was added to the dmso chunk. This heats up a little and liquifies, somewhat, the dmso. Swirl. With vigorous stirring, the dillapiole is dripped into the dmso/sulfuric/nabr mixture, which, btw, is now sodium sulfate, The rate is a slow one, taking about an hour to get it all in, keeping it cool in a bath. yield was about 70%
90%!!
Both of these reactions are very general and can be successfully performed. Methylamine in a pipe is a good way of getting high yields. But heres what swim did; put the undistilled iodo-cmpd in 10x amount of alcohol by wt. Refluxing this for 6 hours gave an eventual yield of DMMDA-2 which is quite rewarding. No one should doubt the power of delepine!
Add HCl until the ph is 2. The red liquid is evaporated until a mass of hard rocklike crystals remained. This is impure DMMDA-2. The crystals CANNOT be cleaned, with ether or any other washes. Freebase and distill to give clear, off colored dmmda-2. The yield is 50 % from the beginning. SWIM got ~12 g at the end. Happy Trails! Contact Us | the Hive Powered by: Ultimate Bulletin Board, Version 5.39a |
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