RA!NER

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I have ipa ok perfect
 

johnholding

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

Curiousonion

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

Curiousonion

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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.
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.
G.Patton
 

Saul

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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.
G.Patton
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
 
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Curiousonion

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

johnholding

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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?
 

ossi

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View attachment 7030
Reaction scheme:
Equipment and glassware:
  • 100 ml round bottom flask;
  • Heating plate;
  • Funnel;
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (250 mL x2, 100 mL x4);
  • 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) 7.6 g;
  • MDP2P (PMK) 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.
4. Concentrated hydrochloric acid (HCl 36% 30 ml) is added to this solution. Than, reaction mixture is refluxed 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 Dampierplease can write someone big scale?
🙏🏼
 
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