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Validation of Delepine and of Halosafrole
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Author Topic: Validation of Delepine and of Halosafrole
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.
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%
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.
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