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

[WillD]

what does it mean to treat with hydrogen chloride gas?

blackchipWith 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.

 

[FredDurst]

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

At best, the same amount as PMK-oil, in the form of hydrochloride, but rather less.

William Dampier@William Dampier - What is the method using HCI and dry Acetone please?

 

[Montecristo]

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.

William Dampier

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.

 

[ymaaah]

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!

MontecristoI think instead of diethyl ether you can use acetate ether, its a good way

 

[WillD]

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

 

[Stretcher5335]

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

William DampierGood day to you first and formost
formic acid + ammonium carbonate ( ammonium formate )
Can that be reacted with methanol for the desired methylammonium formate?

 

[Curiousonion]

I tried this conversion recently, did the nmf with formic acid and pmk reflux for 7 hours. Cooled it down then added the 37% hcl, no reaction since it is acid to acid.
Then started refluxing it, as soon as it went over 84c the mixture started to turn into a brown sludge.
I think its wiser to reflux the hcl at around 60c.

Any one has any experience with this reaction and can help?

Thanks

 

[ossi]

I tried this conversion recently, did the nmf with formic acid and pmk reflux for 7 hours. Cooled it down then added the 37% hcl, no reaction since it is acid to acid.
Then started refluxing it, as soon as it went over 84c the mixture started to turn into a brown sludge.
I think its wiser to reflux the hcl at around 60c.

Any one has any experience with this reaction and can help?

Thanks

Curiousonionhi, you solve this problem meanwhile?

 

[Curiousonion]

hi, you solve this problem meanwhile?

ossi
No, not yet.
Trying the reaction again today but going at 45-55c for 6 hours instead of higher temp for 3 hours.
So far it looks better than the previous reaction, it did not turn into tar although it was not a clear yellow after the 7 hour reflux with formic acid as described by op.

 

[ossi]

No, not yet.
Trying the reaction again today but going at 45-55c for 6 hours instead of higher temp for 3 hours.
So far it looks better than the previous reaction, it did not turn into tar although it was not a clear yellow after the 7 hour reflux with formic acid as described by op.

Curiousonionwould be great if you update here
good luck

 

[Curiousonion]

would be great if you update here
good luck

ossiOn second try I refluxed it with the hcl for 6 hours. It stayed a brown liquid.
I added naoh solution to bring ph up (takes a lot of naoh in order to do that).
Seperated with dcm after, separation has a lot of salt residue in it.
Evaporated the dcm and got left with a brown syropy liquid.
I added some hcl to it to bring ph down and now attempting to crystalize it. (unsuccessfully so far)

 

[ossi]

On second try I refluxed it with the hcl for 6 hours. It stayed a brown liquid.
I added naoh solution to bring ph up (takes a lot of naoh in order to do that).
Seperated with dcm after, separation has a lot of salt residue in it.
Evaporated the dcm and got left with a brown syropy liquid.
I added some hcl to it to bring ph down and now attempting to crystalize it. (unsuccessfully so far)

CuriousonionI'm very curious what the experts will say about this
@William Dampier
@G.Patton

 

[Curiousonion]

Honestly it's not the best method.
There is another rxn writeup on this thread where they use 180 to start on an industrial scale. They distill the formic acid they don't reflux it and I understand why, too much acid to neutralize at the end.
But now I'm having trouble crystalizing it.
I added hcl to the goo then added hot methanol and then poured it into cold acetone and placed it in a freezer. But I doubtvl that would work

 

[ossi]

poured it into cold acetone

Curiousonionin this point no crystallization?

 

[Curiousonion]

in this point no crystallization?

ossiNone what so ever.
Could be due to water residue or dcm residue.
Next I'll try to make some acidic water and see if the mdma freebase gets pulled into it from the dcm and then boil the water off.

 

[Dreadz87]

None what so ever.
Could be due to water residue or dcm residue.
Next I'll try to make some acidic water and see if the mdma freebase gets pulled into it from the dcm and then boil the water off.

CuriousonionHow did this go? Have you made any progress lately brother ?

 

[Camilo]

Would this work for synthetizing MDA from M.Dphenylacetone?

 

[Camilo]

Would this work for synthetizing MDA from M.Dphenylacetone?

CamiloHow would the process and reagents change? Is there a video of this method? Thanks in advance!

 

[G.Patton]

How would the process and reagents change? Is there a video of this method? Thanks in advance!

Camilo>>>How would the process and reagents change?
I already told you about reagents
>>>Is there a video of this method?
there is no video

 

[Camilo]

>>>How would the process and reagents change?
I already told you about reagents
>>>Is there a video of this method?
there is no video

G.PattonThank you for your patience

 

[blitzen.maniax]

Would this work for synthetizing MDA from M.Dphenylacetone?

CamiloJust a wee word of caution if you are using the S isomer for your MDMA that if you decide to go to the MDA product instead then it's the R isomer you need for MDA and the S for MDMA . The good thing is if you plan it right there's no waste

 

[bitcoinup2020]

Hello, I'm a beginner.

I would like to ask about topic 4.
4. Concentrated hydrochloric acid (HCl 36% 30 ml) is added to this solution. Than, reaction mixture is heated at 80 °C for additional 3 h.

Can I use Hydrochloric Acid 35% instead of Hydrochloric Acid 36%?

 

[bitcoinup2020]

Hello, I'm a beginner.

6. Crude MDMA free base is extracted from the alkaline solution with diethyl ether (or petroleum ether) 2 x 50 mL. Ether extract with MDMA free base is dried over MgSO4.

from step 6
What reagents can I use instead of diethyl ether?

Thank you very much for the answer. with respect

 

[chemistry.mob]

How much MDP2P do I need to be able to obtain 1kg of MDMA?
Thank you!!