The Vespiary

The Hive => Methods Discourse => Topic started by: wolfx on August 03, 2001, 05:46:00 PM

Title: Strange distillation problem.
Post by: wolfx on August 03, 2001, 05:46:00 PM

In my previous try, I got my best ketone ever, nice clean yellow, no iso forerun, real nice.
I think I did a bad amination, used large mouth 2.0 l flask, lost too much MeAm, I heated it on low after the heat peak.
When extracting the Al sludge with MeOH and filtering through Celite, the color was dark red. ( I don't think this is the right color, should be yellow/orange, dark ).
Next, MeOH boiled away, A/B, looked normal.
Now the problem, I added peanut oil ( 100 % pure according to label ) and tried to distill the freebase. It took sometime to start distilling, I noticed what looked like a black puff of smoke ( ? ) in the boiling flask. The freebase started distilling, I though I had it, then it slowed down, I kept on increasing the heat, but nothing, when my oil bath started to make smoke I gave up.
Later on I checked my vacuum pump, the vacuum was more than 20 mm Hg, the upper limit of my gauge. I checked the oil, full of black particulate. After flushing and changing the oil, the pump was back to normal. I was tired and frustrated, decided that it was a total loss and not tried to recover the freebase. Later on, I got a few drops left in the condenser and tried it, real nice.

1) Does anybody knows what could have caused it ? The peanut oil ? Some byproduct of the bad amination ?
2) Should I expect something like this to happen again ?
3) Should I wash the freebase prior to distillation ?

Thank you,
W.

Title: Re: Strange distillation problem.
Post by: Osmium on August 04, 2001, 11:19:00 AM

Just a theory:
Vegetable oils are esters of glycerine and fatty acids. Reacting amines with esters produces the amide and the alcohol.

RNH2 + R'-COOR" -----> RNH-CO-R' + R"OH

Congratulations, seems like you are the first scientist who prepared mixed (unsaturated) fatty acid amides of MDMA.  :P

I wouldn't use oils for freebase distillation.

Title: Re: Strange distillation problem.
Post by: wolfx on August 04, 2001, 03:24:00 PM

Thanks Os, real cool. I don't plan to use the peanut oil again.

Title: Re: Strange distillation problem.
Post by: baalchemist on August 04, 2001, 04:58:00 PM

Baal has found that using peanut oil has no advantages when vac distilling, only creates problems. If you have a good vac source any type of buffering agent is unnecessary.

Title: Re: Strange distillation problem.
Post by: Goodtimes on August 04, 2001, 09:59:00 PM

Thanks for the info, saved swim from a possible future fuckup!  ;D

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