09-30-03 00:26
No 461709
Method 1
To a well stirred, cooled mixture of 34g of 30% H202 (hydrogen peroxide) in 150g 80% HCO2H (formic acid) there was added, dropwise, a solution of 32.4g isosafrole in 120ml acetone at a rate that kept the reaction mixture from exceeding 40 deg C. This required a bit over 1 hour, and external cooling was used as necessary. Stirring was continued for 16 hours, and care was taken that the slow exothermic reaction did not cause excess heating. An external bath with running water worked well. During this time the solution progressed from an orange color to a deep red. All volatile components were removed under vacuum which yielded some 60g of a very deep residue. This was dissolved in 60ml of MeOH (methyl alcohol -- methanol), treated with 360ml of 15% H2SO4 (sulfuric acid), and heated for 3 hours on the steam bath. After cooling the mixture was extracted with 3x75ml Et2O (diethyl ether) or C6H6 (benzene). Its recommended that, the pooled extracts can washed -- first with H2O and then with dilute NaOH (sodium hydroxide). Then the solvent is removed under vacuum to afford 20.6g 3,4-methylenedioxyphenylacetone (3,4-methylenedioxybenzyl methyl ketone). The final residue may be distilled at 2.0mm/108-112 deg C, or at about 160 deg C at the water pump.
Add 23g 3,4-methylenedioxyphenylacetone to 65g HCONH2 (formamide) and heat at 190 deg for five hours. Cool, add 100ml H20, extract with C6H6 (benzene) and evaporate in vacuum the extract. Add 8ml MeOH (methyl alcohol -- methanol) and 75ml 15% HCl to residue, heat on water bath two hours and extract in vacuum (or basify with KOH and extract the oil with benzene and dry, evaporate in vacuum) to get 11.7 g 3,4-methylenedioxyamphetamine (MDA).
To produce MDMA substitute N-methylformamide for formamide in the above synthesis.
ive got this formula i dont know if its tru or false one, i just want to know if someone out there would be so nice and help me trough this formula i dont understand the englis very well i have most of the chemicals neded i got dem from my school. im from denmark and i am just sick of the mdma pills that i newer know whats in them so i would like to make the synthesis on my own for my self only. but i neeeeed help so plese once more kan somebody help mewith some details or step by step something like that. pleaseeeeeee.
(Hive Addict)
09-30-03 00:35
No 461710
the first reaction you mention is the old performic. you don't
want to use that. you want to use the "modified" aka. "buffered"
performic or better yet the peracetic method. utfse for details.
the second reaction is the leuckart. as an alternative, search for the
Al/Hg (aluminium amalgam) reaction with methylamine (MeNH3) or
nitromethane (MeNO2). and for god's sake don't use benzene - it
is a strong carcinogen and should not be handled by newbees.
btw: why the fuck do you tell us so much personal details? the police
_is_ reading here too.
n'importe quoi
(Hive Bee)
09-30-03 00:48
No 461713
The procedure you posted is for a leuckart reaction, which will yield MDA as written. Not MDMA, which I assume is what you are after. You could use N-methylformamide in place of formamide in the above reaction however it is not recommended. I would not personally recommend the above synth if this is your first time synth. If you say you have access to formic acid et al. I would suggest looking at rhodiums site (see link at bottom of page) and under Chemistry>Epoxide related>Peracid oxidation of isosafrole to MDP2P follow the synth for a buffered performic, or try Chromic's Propenylbenzene Oxidation to P2P's using Peracetic Acid. These should be easier, more predictable, and higher yielding, with less impurites that may or may not be associated with leuckarts.
I also just posted a procedure for titrating H2O2 Post 461708 (methyl_ethyl: "Failed Peracid Oxidations? Check your H2O2 conc.!!", Newbee Forum) which may be a good idea before preparing your peracid, as said solution seems to degrade over time, which may cause the reaction to fail IMO....
good luck,
m_e
EDIT:: Sorry Hypo, you beat me to it, (I have been having problems posting this for some reason)
Unipolar Mania, It's good for life...
(Newbee)
09-30-03 04:39
No 461745
P has very little chem knowledge,and on the first try succeded with MethylMan's benzoquinone wacker writeup on Rhodium's page,ended up with 120 grams MDP2P,double distilled.Then used LaBTop's borohydride reduction,also on Rhodium's page,with an excess of methylamine and a small excess of sodium borohydride,and redistilled the freebase.Followed the instructions,with a little common sense, and got 70 grams of crystal clear kick ass snow white MDMA. Friends love it,say it's the cleanest.
Probably could have gotten more if P's lab technique were better, but who cares??Next little project is MDA,them P is retired from all this.If you can get the benzoquinone/borohydride,this would be Pooky's suggestion.