The reaction proceeds according to Scheme 1
Formic acid ethyl ester is added to the MDA free base in the flask. Fig 1
The mixture is boiled under reflux for 16 hours. Fig 2
Next, the volatile components are distilled off to obtain an oil. Fig 3
The resulting oil crystallize over time. Fig 4
N-formyl-3,4-methylenedioxyamphetamine dissolved in 150 ml DCM Fig 6
The resulting solution is washed with 100 ml diluted hydrochloric acid Fig 7
Then it is washed with a diluted solution of sodium hydroxide. Fig 8
Wash again with 100 ml diluted hydrochloric acid Fig 9
DCM is dried over sodium sulfate. Fig 10
DCM distilled off Fig 11
After distilling off the DCM, oil remains in the flask. Fig 12
The oil in the flask crystallizes Fig 13
Crystallized N-formyl-3,4-methylenedioxyamphetamine Fig 14
Сrystals are removed from the flask Fig 15
N-formyl-3,4-methylenedioxyamphetamine is ground in a mortar to powder Fig 16
Powder of N-formyl-3,4-methylenedioxyamphetamine Fig 17
Yield after purification is 13.1 g (93.5 %)
The synthesis was carried out according to the publication Alexander Shulgin PiHKAL: A Chemical Love Story (MDMA section)
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
The mixture is boiled under reflux for 16 hours. Fig 2
Next, the volatile components are distilled off to obtain an oil. Fig 3
The resulting oil crystallize over time. Fig 4
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 dissolved in 150 ml DCM Fig 6
Then it is washed with a diluted solution of sodium hydroxide. Fig 8
Wash again with 100 ml diluted hydrochloric acid Fig 9
DCM is dried over sodium sulfate. Fig 10
DCM distilled off Fig 11
After distilling off the DCM, oil remains in the flask. Fig 12
The oil in the flask crystallizes Fig 13
Crystallized N-formyl-3,4-methylenedioxyamphetamine Fig 14
Сrystals are removed from the flask Fig 15
N-formyl-3,4-methylenedioxyamphetamine is ground in a mortar to powder Fig 16
Powder of N-formyl-3,4-methylenedioxyamphetamine Fig 17
Yield after purification is 13.1 g (93.5 %)
The synthesis was carried out according to the publication Alexander Shulgin PiHKAL: A Chemical Love Story (MDMA section)
