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Validation of Delepine and of Halosafrole
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Author Topic: Validation of Delepine and of Halosafrole
egotrip
NewBee posted 02-04-2000 11:38 PM
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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
2) 240 ml dmso
3)18g 93% H2SO4
4)56g NaBr 99%
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.
Add the NaBr and swirl or stir if you have a good enough (BIG) stirbar. Chopping thru the salt is tough.
With vigorous stirring, the dillapiole is dripped into the dmso/sulfuric/nabr mixture, which, btw, is now sodium sulfate,
and insitu HBr.
The rate is a slow one, taking about an hour to get it all in, keeping it cool in a bath.
The mixture , before adding dillapiole, is yellow-orange. The addition of dillapiole decolorizes the mess and then begins a slow progression through the pukey-green, to yellowish, to the legendary burgundy.
Really, its just a really dark yellow. Maybe with a orangishness.
With proper stirring this takes 24 Hrs.
It must always stay cool and stay stirring.
Then add 1L ice dh2o, decant, and the heavy orange syrup doesnt need to be distilled, it is good enough for the next stage...
yield was about 70%
Finkelstein Swap;
Measure out an equimolar amount of Sodium iodide, add 5% to that, and suspend your bromo cmpd in acetone. Heat it, and as it approaches reflux, carefully add small amounts of the iodide salt to mixture. It darkens, and the reaction is a very visual one, and a very malodourous one, as iodine stinks nicely.
Reflux gentle for 30 min..
90%!!
The road forks here, and the real deal is that methylamine reacts awesomely with iodo-derivatives, and hexamethylenetetramine will give the unmethylated derivative via delepine.
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.
in a rb 500, heat and begin adding slight molar xs of hexamine until all is in.
Refluxing this for 6 hours gave an eventual yield of DMMDA-2 which is quite rewarding.
No one should doubt the power of delepine!
THe workup:
Add HCl until the ph is 2.
filter off the ass-load of NH4CL
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!
Osmium
PimpBee posted 02-07-2000 07:22 AM
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There most important part is missing: bioassay.
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