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| Author | Topic: Stove Top MDA via Leukart |
| dpHarma Member |
 posted 11-15-1999 12:45 PM 
After a brief exp. in a test tube, containing ammonium formate, formic acid and distilled MD-P2P, which tube being heated gently with a propane torch for 3 hrs,a few drops of formic acid being added ocassionaly, followed after 3 hrs. by the addition of a few mls. of muriatic acid and vigorous boiling. the contents were basified, extracted with DCM, the DCM washed, then removed leaving a brown oil which when tasted and bioassayed, provided a satisifactory amt. of bitter and psychoactive material. actually about 500mg. of MDMA citrate (from citric acid). no measurements, no careful nothing. just heating. a subsequent exp. using measured amts. of the same materials, heated in a beaker on top of an electric stove with additions of formic acid over 4hrs, followed by hcl hydrolysis also in beaker on stove. yeilded after workup, 4 gms. MDA.hcl from 6 gms. MD-P2P. I never imagined it was this easy. too freakin' much! dpHarma |
| randolph
carter Member |
posted 11-15-1999 03:46 PM
yeah dpharma..... see why i have a fondness for the leu/wall reaction and it's simple elegance.....
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| Atomicdog Member |
posted 11-15-1999 04:21 PM
AD has been trin to push this one lately, even looking hard at the n_Methylformamide snyth for MDMA. One thing, AD has never done this but he thinks that one should basify and extract, then wash the solvent, then acidify and extract with water! This should yield a very clean result. Nice work. |
| Atomicdog Member |
posted 11-15-1999 04:33 PM
Oh... Formic acid + Ammonia -> Ammonium formate AD says, reflux for several hours until the smell changes from one horrible smell to another horrible smell, than evap for crystals or calculate concentration based on ammounts of reactents used. |
| dpHarma Member |
posted 11-16-1999 01:21 PM
evap H2O at low temps as decomposition occurs much above 40^C. too much heat and you will lose yeild. a dehydration cabinet with CaCl2 in a shallow tray with a small fan blowing over it will yeild dry crystals from soup very quickly. the ammonium formate decomposes when heated to produce formamide and water, but some formamide will steam distill off with the water if heated too hard. and if not removed, the water will inhibit the rxn with the ketone (apparently). The rxn described heated the test tube cautiously, with the tip of a propane soldering torch in a clamp allowing precise control, (away from drafts). the formate was 'still wet' crystals, so contained excess water. The liquid after heating the formate was 'simmered' and a small ring of moisture 'pushed' up the tube walls. After 1 hr heating and loss of 1/2 the volume of the liquid in the tube, MD-P2P and 5 ml of 65% formic acid was added, the tube swirled and heating resumed at a lower temp, just enough to keep gas bubbles rising in the liquid. The slight vapour escaping the tube had along with the ketone 'overtones' both formic acid and ammonia 'tones' . kind of drifting hints of both. curious effect. when the smell began to get more ammonia-ish, drops of formic were added. At an arbitrary 3 hr.point, about 5 ml of muriatic acid was added causing the appearance of a white precipitate as a cloudy swirling mass in the brown oily liquid. The ppt. came and went! during heating and finally disappered. OOOps! just remembered. original rxn contained a ml. of ~50% acetic acid. so the ppt may have been some acetate. who knows! After maybe 20 mins. heating the tube was cooled, poured into 25% NaOH
soln. in a sep funnel, shaken, and extracted with DCM. DCM layer washed
and evaped to yeild brown oil with characteristic bitter taste and hideous
buzz on the tongue. citric acid used to neutralize base and test
drive. somebody should have said it was that easy. and take it from me, there really are people who should NOT have easy access to MDA. ouch! owwwieee owwwieee.
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