MDMA synthesis from piperonylmethylketone (PMK/MDP2P) with formic acid

[Curiousonion]

Use acetone if you can't get ether then. Or ipa

 

[RA!NER]

I have ipa ok perfect

 

[Curiousonion]

Make sure you dry it

 

[johnholding]

Anyone had any issues with this method before i proceed to try??

 

[Curiousonion]

At what temperature do you reflux once you add the hcl?

 

[G.Patton]

Read about Boiling point please. You have to reach this point and keep the reaction mixture for 3h. Also, there is written 150-170 °C.

 

[Curiousonion]

Yes but boiling point of formic acid boiling point is 100c and thats for the first step.
So ill assume second step is 150-170c as well.

 

[Saul]

unpossible with HCI
but in this step you dont over heat the flask becouse other wise you get black teer . Check you boiling point by add a small stone in your flask. My guess temp goes max 75°c

only with the use off vacuum, you can raise temp

 

[Curiousonion]

Ah ok, so you recommend to reflux it at 75c?
I don't think it needs such a high temperature with hcl.

 

[G.Patton]

You have to reach boiling. Also, @Saul is right about boiling chips.

 

[Curiousonion]

I usually use stirring when boiling my reactions. I find it's more efficient than boiling stones

 

[G.Patton]

Your stirring bar makes boiling centers like boiling chips.

 

[johnholding]

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.

What temperature do i reflux this at?

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.

Also will there be a video on this method?

 

[G.Patton]

Maintain the temperature when the boiling starts. It named boiling temperature.
probably yes

 

[ossi]

can i have CAS please?

 

[ossi]

please can write someone big scale?

 

[Curiousonion]

Did you try it first scale to see if you can do the rxn first?

 

[ossi]

ofc i try first this scale

 

[Curiousonion]

And how did it go?

 

[ossi]

sorry, my english is not so good, german better. i mean i want try first same as here written, still waiting reagents.
but i'm confident