WillD

Expert
Joined
Jul 19, 2021
Messages
685
Reaction score
965
Points
93
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.
 

Montecristo

Don't buy from me
New Member
Joined
Dec 29, 2021
Messages
102
Reaction score
32
Points
18
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

Don't buy from me
Resident
Joined
Oct 27, 2022
Messages
156
Reaction score
51
Points
28
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

Expert
Joined
Jul 19, 2021
Messages
685
Reaction score
965
Points
93
u can also try to find a methylammonium formate (dry), but not sure if it's available now.
 

Curiousonion

Don't buy from me
Resident
Joined
Aug 29, 2022
Messages
190
Reaction score
66
Points
28
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

Don't buy from me
Resident
Joined
Sep 15, 2022
Messages
69
Reaction score
29
Points
18
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

Don't buy from me
Resident
Joined
Aug 29, 2022
Messages
190
Reaction score
66
Points
28
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

Don't buy from me
Resident
Joined
Sep 15, 2022
Messages
69
Reaction score
29
Points
18
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

Don't buy from me
Resident
Joined
Aug 29, 2022
Messages
190
Reaction score
66
Points
28
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

Don't buy from me
Resident
Joined
Sep 15, 2022
Messages
69
Reaction score
29
Points
18
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

Don't buy from me
Resident
Joined
Aug 29, 2022
Messages
190
Reaction score
66
Points
28
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
 

Curiousonion

Don't buy from me
Resident
Joined
Aug 29, 2022
Messages
190
Reaction score
66
Points
28
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

Don't buy from me
New Member
Joined
Jan 3, 2023
Messages
2
Reaction score
0
Points
3
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

Don't buy from me
New Member
Joined
Jan 7, 2023
Messages
16
Reaction score
2
Points
3
Would this work for synthetizing MDA from M.Dphenylacetone?
 

Camilo

Don't buy from me
New Member
Joined
Jan 7, 2023
Messages
16
Reaction score
2
Points
3
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

Expert
Joined
Jul 5, 2021
Messages
2,587
Solutions
3
Reaction score
2,618
Points
113
Deals
1
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
 

blitzen.maniax

Don't buy from me
New Member
Joined
Feb 4, 2024
Messages
1
Reaction score
2
Points
3
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

Don't buy from me
Resident
Joined
Jan 12, 2023
Messages
58
Reaction score
16
Points
8
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%?
 

2-79-790125

Don't buy from me
Member
Joined
May 26, 2024
Messages
82
Reaction score
21
Points
8
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%?
bitcoinup2020bitcoinup2020
I have never successfully made any MDMA but in my research HCl 35% vs HCl 36% has no significant difference at all for any MDMA synthesis. We are fortunate that it doesn't require that exact of tolerances. To be clear, I am a complete Rookie with limited experience and this is my opinion.
 

bitcoinup2020

Don't buy from me
Resident
Joined
Jan 12, 2023
Messages
58
Reaction score
16
Points
8
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

Don't buy from me
New Member
Joined
Mar 12, 2023
Messages
80
Reaction score
34
Points
18
How much MDP2P do I need to be able to obtain 1kg of MDMA?
Thank you!!
 
  • Free product samples

    Testing products from new vendors and manufacturers.

    Get free samples for testing now!

  • Always stay in touch with BB forum. Element/Matrix.

    Connect notifications to always stay in touch with the forum!

    Connect

Top