Synthesis of N-formyl-3,4-methylenedioxyamphetamine (Precursor for MDMA Synthesis)

GhostChemist

Expert
Joined
Nov 20, 2022
Messages
220
Reaction score
363
Points
63
The reaction proceeds according to Scheme 1
PSYmBJOgCa


Download Video

Starting Reagents and Materials

  • 24 g MDA (free base)
  • 50-55 ml Formic acid ethyl ester (ethyl formate CAS 109-94-4)
  • 100 ml flask
  • Beakers
  • Reflux condenser
  • Heater with stir

Synthesis

Formic acid ethyl ester is added to the MDA free base in the flask. Fig 1
1ov5T6aJI7

The mixture is boiled under reflux for 16 hours. Fig 2
E4cDxVBgdj

Next, the volatile components are distilled off to obtain an oil. Fig 3
ZaIRqsdjiF

The resulting oil crystallize over time. Fig 4
P7lNWmH3qb

Yield 28.1 g (the yields also do not correspond to stoichiometry similar to Shulgin's prescription, possibly due to impurities; when recalculated through purified formyl, the yield is ~94%)

Purification

Starting Reagents and Materials

  • 14 g N-formyl-3,4-methylenedioxyamphetamine
  • 150 ml DCM
  • 200 ml 3-3.5% HCl
  • 5 g NaOH in 100 ml H2O
  • 10-15 g anhydrous Na2SO4
  • Distillation unit
  • Separatory funnel
  • Flasks
  • Beakers
N-formyl-3,4-methylenedioxyamphetamine for further purification Fig 5
L6HpmFUdWQ

N-formyl-3,4-methylenedioxyamphetamine dissolved in 150 ml DCM Fig 6
ElqfJCA7Qn

The resulting solution is washed with 100 ml diluted hydrochloric acid Fig 7
2XZNLSYkfb

Then it is washed with a diluted solution of sodium hydroxide. Fig 8
Iblm0VB9PF

Wash again with 100 ml diluted hydrochloric acid Fig 9
VuIFh8yqto

DCM is dried over sodium sulfate. Fig 10
O6SQMdpANE

DCM distilled off Fig 11
UEOkBlJWzT

After distilling off the DCM, oil remains in the flask. Fig 12
WdFOhPbDIn

The oil in the flask crystallizes Fig 13
GILOZkFBop

Crystallized N-formyl-3,4-methylenedioxyamphetamine Fig 14
TpNIasKOGh

Сrystals are removed from the flask Fig 15
KRdVPqvspg

N-formyl-3,4-methylenedioxyamphetamine is ground in a mortar to powder Fig 16
SEaXtoIsxm

Powder of N-formyl-3,4-methylenedioxyamphetamine Fig 17
9dhBU0Y68D

Yield after purification is 13.1 g (93.5 %)

Source

The synthesis was carried out according to the publication Alexander Shulgin PiHKAL: A Chemical Love Story (MDMA section)
 

Attachments

  • yFQMB2zr4j.jpg
    yFQMB2zr4j.jpg
    456.4 KB · Views: 14
  • WvJFQi26Rd.jpg
    WvJFQi26Rd.jpg
    420.7 KB · Views: 15
Last edited by a moderator:

loadingST

Don't buy from me
Resident
Language
🇧🇬
Joined
Sep 10, 2023
Messages
190
Reaction score
108
Points
43
Can i ask why someone woud need the n-formyl derivate of mda ? To transport as legal substitute?
 

GhostChemist

Expert
Joined
Nov 20, 2022
Messages
220
Reaction score
363
Points
63
N-formyl-3,4-methylenedioxyamphetamine is a direct derivative of MDA, this information must be in the laws.
But after reduction of N-formyl-3,4-methylenedioxyamphetamine with NaBH4, not formed the MDMA, but formed intermediate substance may be not controlled and in the next stage can be convert in mdma with LAH reduction (But note it is important! The process formation of MDMA must be confirm experimentally in future)
 

ukises

Don't buy from me
Member
Language
🇪🇸
Joined
Feb 6, 2025
Messages
28
Reaction score
4
Points
3
This way like easy

The Method of Decker and Becker[53]

179 g (1 mole) of MDA as the free base and 106 g (1 mole) of benzaldehyde are dissolved in 95% ethanol (as much it takes to dissolve them). This solution is refluxed for 30 minutes forming the Shiff base (imine) intermediate of these two compounds. The ethanol is removed by distilling under reduced pressure leaving an oil.

This oil is added to 142 g (1 mole) of methyl iodide and placed in a pipe "bomb". Use a pipe with fine threads and wrap these with teflon tape to form a good seal. Tighten down the caps well and place the pipe "bomb" in boiling water for five hours. The material in the "bomb" is then washed out with a solution of 80ml methanol and 10 ml water and placed in a boiling flask to be refluxed. Only enough solution to rinse out the pipe is required. Reflux the mixture for 30 minutes. Add an equal volume of water and reflux the mixture until the odor of benzaldehyde has disappeared. Acidify the mixture with hydrochloric acid (shake well) and the extract with three portions of ether. The solution is made basic with 25% NaOH solution and the liberated amine is extracted with ether (or methylene chloride etc.). The ether is washed with water, dried with MgSO4 and HCl gas is run into the solution to precipitate the amine. Filter and allow to dry.

The MDMA may contain some MDA but this should be acceptable. Replacing methyl iodide with 156g (1 mole) ethyl iodide and boiling the pipe for 10-15 hours will give Eve.
 

the money

Don't buy from me
Resident
Language
🇺🇸
Joined
Nov 26, 2022
Messages
60
Reaction score
36
Points
18
Thank you very much for your effort

Please publish the sequel and videos as soon as possible.
🌹🌹🌹
 
Top