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Synthesis of MDMA from piperonylmethylketone (PMK) with Formic acid

William Dampier

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Reaction scheme:
GS1xjmHMBd


Synthesis:
1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
5. 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.
6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.
 
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Honolulu98

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Reaction scheme:
View attachment 1473

Synthesis:
1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
5. 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.
6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.
if possible use DMF or is better NMF?


Any difference?
 

William Dampier

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No, DMF is impossible for this reaction
 

rickyrick

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What in your opinion is the best way to get or synthesise PMK at this day and age?PMK methyl glycidate maybe?
 

William Dampier

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Definitely PMK-gly is the best source (after sassafras oil, if you can buy it)
 
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Gale

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This method seems really nice, but how are the yeilds?
 

blackchip

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what does it mean to treat with hydrogen chloride gas?
 

William Dampier

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what does it mean to treat with hydrogen chloride gas?
With a gas generator. But you can use aqueous hydrochloric acid and dry acetone.
This method seems really nice, but how are the yeilds?
At best, the same amount as PMK-oil, in the form of hydrochloride, but rather less.
 

Followme38

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Can you use standard formamide instead of nmf ?
 

blackchip

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With a gas generator. But you can use aqueous hydrochloric acid and dry acetone.

I am sorry for asking this question again but I read the literature on the hcl gas generator but it doesn't answer my question. If I make the gas with the generator, does 'treating' mean passing the gas through a flask with the crude MDMA?
 

Followme38

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I am sorry for asking this question again but I read the literature on the hcl gas generator but it doesn't answer my question. If I make the gas with the generator, does 'treating' mean passing the gas through a flask with the crude MDMA?
Just use anhydrous acetone and 37% hcl working with hcl gas is dangerous as hell :( and there is not advantage if you crystal in fridge
 

Gale

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Just use anhydrous acetone and 37% hcl working with hcl gas is dangerous as hell :( and there is not advantage if you crystal in fridge
You mean to add 37% hcl dropwise to anhydrous acetone till acidic then freeze? Gassing isn't that dangerous if done properly, its really chill. Just not the most comfortable, I would rather have a dry acidic solution I could add to the NP, such as sulfuric acid. Would be smoother. Will it be ok to go the sulphate route? I have a feeling it will make some pretty crystals ;)
 
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Followme38

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You mean to add 37% hcl dropwise to anhydrous acetone till acidic then freeze? Gassing isn't that dangerous tbh and with proper exhaust you can even take your mask off.

Gassing seems to be the best option and will cut down on time and solvents.
You are right at this point only its hard to get your hands on gas most of the time :)
 

Gale

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You are right at this point only its hard to get your hands on gas most of the time :)
Unless you live in most places where its the easiest reagent to access. HCL aq poured on calc chloride = gasolina
 

Montecristo

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hey, What is the formic acid concentration?
So instead of gassing i would wash the residue with hcl and acetone?
Is there alternative to diethyl ether? can i use DCM? or Naptha?
And do i have to convert the new [Ethyl Gylc] PMK into PMK oil?
Thanks!
Reaction scheme:
View attachment 1473

Synthesis:
1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
5. 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.
6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.


Reaction scheme:
View attachment 1473

Synthesis:
1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
5. 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.
6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.
 

Montecristo

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How much hcl and dry acetone should be used?
what is yeild compared to bubbling hcl?
 

Gale

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How much hcl and dry acetone should be used?
what is yeild compared to bubbling hcl?
Yeild should be the same and IMO gassing is the best method whether you perform this step directly or after collecting and drying out base, then dissolve in IPA and maybe add a few mls hcl aq and freeze..which should give you some crystals..but id reccomend to gas a bunch of IPA and save it. Then you have dry IPA/HCL. Whenever you need it, its ready and all you have to do is add HCl/IPA to dry NP to pH 5?

The gassing stage is really the most relaxing step. It seems intimidating but with good exhaust airflow you don't even need to wear a mask IME, I take mine off sometimes and I dont smell a thing...might be smart to wear protective face sheild for w.e reason the tube gets clogged and pressure builds up and escapes in random direction.
 

Gale

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How much hcl and dry acetone should be used?
what is yeild compared to bubbling hcl?
Yeild should be the same and IMO gassing is the best method whether you perform this step directly or after collecting and drying out base, then dissolve in IPA and maybe add a few mls hcl aq and freeze..which should give you some crystals..but id reccomend to gas a bunch of IPA and save it. Then you have dry IPA/HCL.. IMO it feels more organised to me when using dry IPA/hcl..no need for setting up for gassing or waiting for the right time to gas etc.

The gassing stage is really the most relaxing step. It seems intimidating but with good exhaust airflow you don't even need to wear a mask IME, I take mine off sometimes and I dont smell a thing...might be smart to wear protective face sheild for w.e reason the tube gets clogged and pressure builds up and escapes in random direction, which could blind u or give u a nice burn... With that in mind, gassing is still a relaxing and easy process.
 

Montecristo

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Yeah sweet, i am aware of how to gas HCL to get a higher concentration acid using Azeotrope distillation, is this the same method with the gas line going into solution?
 

Montecristo

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do you just gas until all the product has crystalized?
 
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