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

[Followme38]

Can you use standard formamide instead of nmf ?

 

[CryoThio]

Can you use standard formamide instead of nmf ?

Followme38It will produce MDA, not MDMA, but yes, you can. The methyl group is necessary for mdma

 

[Jasonmorales77]

It will produce MDA, not MDMA, but yes, you can. The methyl group is necessary for mdma

CryoThioCould i generate MDA with this route changing something can someone explain me how?

 

[CryoThio]

Could i generate MDA with this route changing something can someone explain me how?

Chemistking77There should be some write ups on here.

Mda is produced by reacting formamide with mdp2p.

Mdma is produced by reacting n methyl formamide with mdp2p.

 

[Camilo]

Would this work for synthetizing MDA from M.Dphenylacetone?

 

[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

 

[ZACARIASKLK123]

The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.

7.32 g in total, added as whole in one step?
or
7.32 g of formic acid, additions divided over 7h using a drip funnel?

 

[The FALCON]

View attachment 7030
Reaction scheme:

View attachment 1473
​

Equipment and glassware:

• 100 ml round bottom flask;​
• Retort stand and clamp for securing apparatus (optional);​
• Reflux condenser;​
• Heating plate;​
• Funnel;​
• Syringe or Pasteur pipette;​
• pH indicator papers;​
• Beakers (250 mL x2, 100 mL x4);​
• Vacuum source;​
• Laboratory scale (0.01-100 g is suitable);​
• Measuring cylinders 10 mL and 100 mL;​
• Water bath;​
• Glass rod and spatula;​
• Separatory funnel 0.5 L;​
• Laboratory grade thermometer (up to 200-250 °C); ​
• Buchner flask and funnel; ​
• Filter paper;​

Reagents:

• Formic acid 10.98 g;​
• n-Methylformamide (NMF; cas 123-39-7) 7.6 g;​
• MDP2P (PMK; cas 4676-39-5) 9.0 g;​
• Concentrated hydrochloric acid (HCl 36%) 30 ml;​
• Sodium hydroxide solution (NaOH 35%) ~10 ml;​
• Diethyl ether (or petroleum ether) ~150 ml;​
• Magnesium sulphate (MgSO4) ~15 g;​
• Methanol (MeOH) ~50 ml;​
• Acetone ~50 ml;​

Synthesis:

1. Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
2. The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
3. After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained. N-formyl-MDMA solution have to be washed with distilled water twice and dried over MgSO4. Dry solution is filtered from solids.
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.
5. The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
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.
7. After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
8. The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
9. MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.​

William DampierMdp2p should be oil or powder at first ?if oil how to convert powder to oil ?

 

[The FALCON]

View attachment 7030
Reaction scheme:

View attachment 1473
​

Equipment and glassware:

• 100 ml round bottom flask;​
• Retort stand and clamp for securing apparatus (optional);​
• Reflux condenser;​
• Heating plate;​
• Funnel;​
• Syringe or Pasteur pipette;​
• pH indicator papers;​
• Beakers (250 mL x2, 100 mL x4);​
• Vacuum source;​
• Laboratory scale (0.01-100 g is suitable);​
• Measuring cylinders 10 mL and 100 mL;​
• Water bath;​
• Glass rod and spatula;​
• Separatory funnel 0.5 L;​
• Laboratory grade thermometer (up to 200-250 °C); ​
• Buchner flask and funnel; ​
• Filter paper;​

Reagents:

• Formic acid 10.98 g;​
• n-Methylformamide (NMF; cas 123-39-7) 7.6 g;​
• MDP2P (PMK; cas 4676-39-5) 9.0 g;​
• Concentrated hydrochloric acid (HCl 36%) 30 ml;​
• Sodium hydroxide solution (NaOH 35%) ~10 ml;​
• Diethyl ether (or petroleum ether) ~150 ml;​
• Magnesium sulphate (MgSO4) ~15 g;​
• Methanol (MeOH) ~50 ml;​
• Acetone ~50 ml;​

Synthesis:

1. Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
2. The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
3. After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained. N-formyl-MDMA solution have to be washed with distilled water twice and dried over MgSO4. Dry solution is filtered from solids.
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.
5. The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
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.
7. After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
8. The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
9. MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.​

William DampierBy what can i replace hcl gas ?

 

[hider8028]

Is MDP2P oil right? How is 9Gram?

 

[Tegridy]

View attachment 7030
Reaction scheme:

View attachment 1473
​

Equipment and glassware:

• 100 ml round bottom flask;​
• Retort stand and clamp for securing apparatus (optional);​
• Reflux condenser;​
• Heating plate;​
• Funnel;​
• Syringe or Pasteur pipette;​
• pH indicator papers;​
• Beakers (250 mL x2, 100 mL x4);​
• Vacuum source;​
• Laboratory scale (0.01-100 g is suitable);​
• Measuring cylinders 10 mL and 100 mL;​
• Water bath;​
• Glass rod and spatula;​
• Separatory funnel 0.5 L;​
• Laboratory grade thermometer (up to 200-250 °C); ​
• Buchner flask and funnel; ​
• Filter paper;​

Reagents:

• Formic acid 10.98 g;​
• n-Methylformamide (NMF; cas 123-39-7) 7.6 g;​
• MDP2P (PMK; cas 4676-39-5) 9.0 g;​
• Concentrated hydrochloric acid (HCl 36%) 30 ml;​
• Sodium hydroxide solution (NaOH 35%) ~10 ml;​
• Diethyl ether (or petroleum ether) ~150 ml;​
• Magnesium sulphate (MgSO4) ~15 g;​
• Methanol (MeOH) ~50 ml;​
• Acetone ~50 ml;​

Synthesis:

1. Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
2. The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
3. After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained. N-formyl-MDMA solution have to be washed with distilled water twice and dried over MgSO4. Dry solution is filtered from solids.
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.
5. The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
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.
7. After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
8. The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
9. MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.​

William Dampierhow long would this process take on average?

 

[WillD]

how long would this process take on average?

TegridyThis process can be divided into two stages (and two days) getting the result on the third day. But you can scale in quantity. We will edit the published synthesis in the future to increase productivity (using additional water in the reaction).

 

[mickael1985]

Hello
What quantities of acetone and chloridric acid should it be added to the MDMA Freebase Oil? How to extract acid and acetone then? I am not a chemist thank you for explaining to me in consequence.

 

[WillD]

Hello
What quantities of acetone and chloridric acid should it be added to the MDMA Freebase Oil? How to extract acid and acetone then? I am not a chemist thank you for explaining to me in consequence.

mickael19855:1 acetone:aq.hcl~37% at min. After crystallizes in the freezer at least a day, if you have no experience. After filtration, leave the sediment and continue to crystallize it.