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Synthesis of MDMA from piperonylmethylketone (PMK) with formamide and LAH

William Dampier

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RpsDHNMr5E

1. Formamide (65 g) and PMK (23 g) were refluxed at 190 *C for 5 h.
2. The solution was made basic and extracted with diethyl ether.
3. The ethereal solution was washed with dilute sulphuric acid, rinsed with water and finally dried over anhydrous sodium sulphate.
4. The diethyl ether volume was reduced to yield a clear yellow solution of N-formyl-3,4-methylenedioxyamphetamine (N-formylMDA).
5. This was added dropwise to LAH (2,5 g in 100 ml of sodium-dried diethyl ether) and refluxed for 3 h.
6. The excess LAH was decomposed by the addition of water and the resulting mixture was filtered, and the precipitate washed with diethyl ether.
7. The washings and the filtrate were combined and extracted with dilute sulphuric acid.
8. The aqueous solution was made alkaline with dilute sodium hydroxide and extracted with diethyl ether
9. The solvent was evaporated, leaving an amber oil of crude MDMA.
10. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
 
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DeepSpace9

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Would you care to go over some of these steps in layman? as well as tools?
2) "made basic" by adding basic salts? to lower the ph? extracted using what tool?
3) the process requires what equipment to dry over anhydrous sodium sulphate? How does this look visually?
I suppose I must request a direct message, most of this can be better understand knowing what equipment is needed to perform the functions.

Forgive my lack of proper education.
 

G.Patton

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Don't be sorry :)
"made basic" by adding basic salts?
You have to add base solution such as NaOH/KOH solution in water (~40%), use pH indicator to cheek pH (~12 is appropriate).
dry over anhydrous sodium sulphate
You have to add anhydrous sodium sulfate to organic solution. This substance will absorb water remains from organic solvent.

Moreover, look at Laboratory FAQ part, there are a lot of information to learn. It will help you!
 
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DeepSpace9

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Sweet! Thank you,
would you by chance have a list of lab equipment that would be needed for this pmk conversion? :)))) :)
 

DeepSpace9

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Would you care to share a list of equipment needed for this? From scratch?
 

Gale

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Sounds clean. May I ask what was the yeild? If I remember correctly this is an old synth
 

Montecristo

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View attachment 1472
1. Formamide (65 g) and PMK (23 g) were refluxed at 190 *C for 5 h.
2. The solution was made basic and extracted with diethyl ether.
3. The ethereal solution was washed with dilute sulphuric acid, rinsed with water and finally dried over anhydrous sodium sulphate.
4. The diethyl ether volume was reduced to yield a clear yellow solution of N-formyl-3,4-methylenedioxyamphetamine (N-formylMDA).
5. This was added dropwise to LAH (2,5 g in 100 ml of sodium-dried diethyl ether) and refluxed for 3 h.
6. The excess LAH was decomposed by the addition of water and the resulting mixture was filtered, and the precipitate washed with diethyl ether.
7. The washings and the filtrate were combined and extracted with dilute sulphuric acid.
8. The aqueous solution was made alkaline with dilute sodium hydroxide and extracted with diethyl ether
9. The solvent was evaporated, leaving an amber oil of crude MDMA.
10. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
Any precautions around LAH on a bigger scale? eg around adding water to it?
would this work well 10x in a 2000ml flask?
On a 10x scale could i put the remaining residue on a pyrex dish and mix with HCL 32% and IPA and freeze precipitate?
Any major safety concerns with any of this procedure?
Expected yields?
 
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William Dampier

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Any precautions around LAH on a bigger scale? eg around adding water to it?
would this work well 10x in a 2000ml flask?
On a 10x scale could i put the remaining residue on a pyrex dish and mix with HCL 32% and IPA and freeze precipitate?
Any major safety concerns with any of this procedure?
Expected yields?
High fire hazard in moisture conditions. Some solvents in this synthesis can be replaced, for greater safety. But then for synthesis it is necessary to add distillation in some stages (stage 2-4). You can extract with ether, but the reaction with LAH is made in the THF or 1,4-dioxane. The volume of the flask, I would not use more than 10L. No matter how modified the reaction, the main task - is to avoid moisture. Perfectly dry equipment, dry air in the room and a fire extinguisher at hand. If you are ready for this reaction, you can write in a private message, I will advise in detail. Also, you can write questions here.
 
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