Sciencemadness Discussion Board

Ethyl formate MDA>MDMA

overunity33 - 29-4-2010 at 00:13

interested in Shulgins MDA>MDMA
Quote:

Holding at reflux for 16 h a solution of 10 g of MDA as the free base in 20 mL fresh ethyl formate. Removal of the volatiles yielded an oil that set up to white crystals, weighing 7.8 g. (MDMA freebase)


Anyone have any advice, information on this?

What about a synthesis for ethyl formate? Will formic acid+ethanol work? What are the reaction parameters?

Nicodem - 29-4-2010 at 01:16

That is a formylation and not a methylation. The product is therefore the corresponding N-alkylformamide, that is N-(1-(benzo[d][1,3]dioxol-5-yl)propan-2-yl)formamide.

PS: If you refuse to use references, open threads in the Beginnings section where this is moved. Also because, if you would have read the original reference (PiHKAL #MDMA) you would have realized that it is about formylation by yourself rather than bothering others.

not_important - 29-4-2010 at 01:55

And a minute or so of Internet searching gives


A treatise on chemistry, Volume 3, Part 1
By Henry Enfield Roscoe, Carl Schorlemmer
Quote:
A still more simple method is to heat anhydrous glycerin with equal molecules of alcohol and oxalic acid, connecting the flask with a reversed condenser until complete decomposition has occurred ; the oxalic acid then requires to be warmed and the ether distils over. The distillate obtained according to one or other of these methods is shaken up with milk of lime in order to remove free acid, and then dried over chloride of calcium and rectified.

According to Dittmar the product thus obtained is, however, not quite pure. In order to remove the impurities it must be warmed for some time with anhydrous copper sulphate and then distilled.



Other possibly useful references

http://www.archive.org/details/practicaltreatis00deitrich

http://www.archive.org/details/alcoholitsproduc00simmuoft


and two modern ones:


http://www.springerlink.com/content/n6wr58333825756w/

http://dx.doi.org/10.1016/S0926-860X(98)00345-7