Synthesis of MDMA from ethyl vanillin


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Jan 10, 2023
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An OTC MDMA synthesis route.​


Even though many routes exist for the synthesis of MDMA but in some routes the precursors are not easily obtainable (like safrole,palladium catalysts,etc), in some routes scalability is an issue (like if you start from vanillin/eugenol as a precursor scalability will totally be an issue let alone bad yields). This route which we are about to discuss should take care of such problems.
The synthesis starts from:- Ethyl vanillin->Protocatechualdehyde->piperonal->PMK glycidate->MDP2P->MDMA
  1. Ethyl Vanillin-> Protocatechualdehyde
Ethyl vanillin is our precursor of choice because it's readily available OTC, is cheap, easier to demethylate than normal vanillin. You basically have to heat it with some sulfuric acid for about an hour at 100°C. Here is a detailed Science Madness post covering this reaction.
2. Protocatechualdehyde-> Piperonal
After we've obtained our Protocatechualdehyde, we methylenate it with DCM in DMSO in the presence of NaOH. Here is a detailed Science Madness post covering this reaction.
3. Piperonal-> PMK glycidate
Now comes the interesting part, credit goes to u/The13chemist for mentioning this reaction in a comment. Now here's the thing, we perform a Darzens Condensation on Piperonal by reacting it with alpha-chloro propionic acid ethyl ester. The reagent might sound intimidating but can be easily produced with simple OTC chemicals. To make the alpha-chloro propionic acid ethyl ester, we first make the propionic acid by reacting calcium propionate (common food additive) with sulfuric acid. After we've got the propionic acid we alpha-chlorinate it with TCCA(pool chemical). After we've got the alpha-chloro propionic acid we make its ethyl ester by dissolving it in ethanol and bubbling dry HCl gas through it.
The overall synthesis of alpha-chloro propionic acid ethyl ester is discussed in this science madness post
Now we react the alpha-chloro propionic acid ethyl ester with piperonal under the presence of NaOEt.
We've now obtained the PMK glycidate.
4. PMK glycidate-> MDP2P
This is easy, all we have to do is reflux the PMK glycidate in HCl, we should get the MDP2P
Sadly this part of the synthesis is not very OTC, since you still have to use traditional methods for the reduction like reducing with NaBH4 or Al/Hg amalgam.
But there is still a method that would be fairly OTC, but it hasn't Been tried and tested popularly, we can use sodium dithionite to reduce the imine.
This is a rhodium page for reference.
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