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Montecristo

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This is one of the classic routes, everything works

Anhydrous formic acid u are unlikely to find. The reaction can be carried out without it, only with N-MethylFormamide
William Dampierawesome thank you!
Would this method scale up safely? eg 10x or 20x?
 

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awesome thank you!
Would this method scale up safely? eg 10x or 20x?
thatfellonEven more. But I'd rather edit the proportions depending on how much PMK you do. For a large and small scale, the proportions may differ, in addition, there are a couple more features, such as the water content of solvents. If you have all the reagents, I am ready to help in PM, you can publish the results here, if you want
 

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u can also try to find a methylammonium formate (dry), but not sure if it's available now.
 

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How much is the yield of that synth finally?
Thanks.
 

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This is one of the classic routes, everything works

Anhydrous formic acid u are unlikely to find. The reaction can be carried out without it, only with N-MethylFormamide
William Dampierbut a non anhydrous formic acid would work?
 

Montecristo

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awesome thank you. I would want to do 90-100g pmk. I do not have the reagents yet , i am waiting on other ones for amphetamine sulfate then i will get onto the reagents needed for this. I will let you know, and i will document both synths and post here for everyone.
Even more. But I'd rather edit the proportions depending on how much PMK you do. For a large and small scale, the proportions may differ, in addition, there are a couple more features, such as the water content of solvents. If you have all the reagents, I am ready to help in PM, you can publish the results here, if you want
William Dampier
 

Montecristo

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first time i will do the synth size as above to get a better understanding/experience , but then i would want to do 10x .
 

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daqwen

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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.
William DampierWhat are the volume measurements of each one?
 

Fring

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awesome thank you. I would want to do 90-100g pmk. I do not have the reagents yet , i am waiting on other ones for amphetamine sulfate then i will get onto the reagents needed for this. I will let you know, and i will document both synths and post here for everyone.
thatfellonplease bro.. kindly post here the results and the proccedure... i want to try this method as well, but since there are not much clear info would be freat if you can help us.
 

ADATA

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Can 28281-49-4 be used as PMK?
 

daqwen

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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.
William DampierWhat NMF means?
 

PepitoPistol

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first time i will do the synth size as above to get a better understanding/experience , but then i would want to do 10x .
thatfellonDid you try this?
Can you share some results? I’m deciding which way to go, but there’s too little info…
Thanks!
 

daqwen

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Can someone explain me the instrucion 5 and 6? Can Somenone explain with more details?
 

MadHatter

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Can someone explain me the instrucion 5 and 6? Can Somenone explain with more details?
daqwen5. 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.

Organic solvents can mostly be evaporated by low heating. It means you reduce the volume of the remaining solution by gentle heating. When you're left with something like half the original volume, you set up a HCl gas generator. This is done by dripping concentrated sulphuric acid onto table salt and passing the fumes that are produced (dry HCl gas) via a tube into the solution to bubble. You can find a detailed description of how to construct a HCl gas generator under "laboratory techniques" on this forum.
Once the HCl gas bubbles into the solution, a brown gel is formed: this is the product. Once no more goo is being formed when you bubble gas into the solution, the reaction is finished and you can filter out the brown goo.

6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.

The "crude salt" is the brown goo. Pour it into some boiling methanol under stirring. When all is dissolved, let chill down for a bit and then pour the mix into ice cold acetone. NOW you'll get the nice MDMA crystals.
 

MadHatter

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Also, before you pour everything into ice cold acetone, make sure it's well below 50 degrees C. Acetone boils at 56 degrees, and if you dump a boiling hot solution into it ...
NW6SuXIVH3
 

IM BATMAN

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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.

Organic solvents can mostly be evaporated by low heating. It means you reduce the volume of the remaining solution by gentle heating. When you're left with something like half the original volume, you set up a HCl gas generator. This is done by dripping concentrated sulphuric acid onto table salt and passing the fumes that are produced (dry HCl gas) via a tube into the solution to bubble. You can find a detailed description of how to construct a HCl gas generator under "laboratory techniques" on this forum.
Once the HCl gas bubbles into the solution, a brown gel is formed: this is the product. Once no more goo is being formed when you bubble gas into the solution, the reaction is finished and you can filter out the brown goo.

6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.

The "crude salt" is the brown goo. Pour it into some boiling methanol under stirring. When all is dissolved, let chill down for a bit and then pour the mix into ice cold acetone. NOW you'll get the nice MDMA crystals.
DocXcould you please explain me more about the cilled acetone? would not be enough put the goo in saturated solution solvent, the wait to cristalize?
tnx!
 
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