caesare.robot

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for further re-crystallisation/purification or if/when someone overacidified and has trouble to get crystals
 

Win Win

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Introduction
The following method shows that the NaBH4 reduction actually is superior to all other common routes used in clandestine chemistry and this method allows to scale MDMA synthesis unlike aluminum amalgam reduction. The method is quite simple, it doesn't take expensive equipment. Procedures with the reaction mixture are simple and efficient. This method is very usefull for big scale production of MDMA and gives high yields (90%+).

There is a relatively fast formation of the imine and the imine is reduced rapidly. There's no reduction of the ketone to the secondary alcohol. In similar reactions, the water that is produced during the forming of the imine (Schiff Base) is removed from the reaction before the imine is reduced with drying salt, or molecular sieves, or by using toluene as the solvent, so the water and the toluene form an azeotrope.

Difficulty rating: 5/10 View attachment 8290

Reagents:
  • Methylamine gas (MeNH2) 300 g;
  • Methanol (MeOH) 3000 g;
  • 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; cas 4676-39-5) 1000 g;
  • Sodium borohydride (NaBH4) 100 g;
  • Distilled water (H2O) 8 L;
  • Hydrochloric acid 8 mL 33% HCl;
  • Dichloromethane (DCM) 200 mL;
  • Acetone 4 L;
  • Sodium hydroxide aq solution 30% (NaOH aq) 200 mL;
Equipment and glassware:
  • Reactor 20 L, equipped with thermometer and overhead stirrer;
  • Freezer;
  • Retort stand and clamp for securing apparatus;
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (2 L x2, 1 L, 500 mL x2);
  • Bucket 20-30 L;
  • Vacuum source;
  • Laboratory scale (1-1000 g is suitable);
  • Measuring cylinders 1000 mL and 100 mL;
  • Cold water bath;
  • Glass rod and spatula;
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
  • Wet towel;
  • Vacuum distillation kit;
  • HCl gas source;
  • Hose (optional);
  • Heating plate or heating mantle;
Procedures
Reagents preparation
Methylamine gas (MeNH2) 300 g is dissolved in chilled 3000 g methanol (MeOH; -17-20 °C) in 20 L reactor, equipped with thermometer and overhead stirrer. The mixture is cooled down to 5 °C. The stirrer is turned on and MDP2P 1000 g is added.
Notes: Methylamine (MeNH2) gas 300 g is made by reaction of methylamine hydrochloride (MeNH2*HCl) with sodium hydroxide (NaOH).

MDP2P reduction to MDMA
Sodium borohydride (NaBH4) 100 g is added in portions, one teaspoon per ~5 min, H2 gas bubbling has to disappear before next addition (wash down with methanol). Temperature is maintain between 8-10 °C. Sodium borohydride (NaBH4) addition is taken 2-7 h. The mixture is stirred for 2 days. The stirring time can be reduced to 4 h for people in a hurry, 10-20% will be lost.
Notes: When the reaction vessel is opened it should be covered by a wet towel, so that the methylamine gas can be absorbed by the water. 1 L Water can absorb 1000 L NH3 gas. An airlock can be used for that goal as well. Do not airtight the flask, let a thin hose out the window (or a fume hood), wrapped at the end with a wet towel.


Distilled water (H2O) 8 L with 8 mL 33% HCl is added to the reaction mixture with a constant stirring. Reaction mixture is turned to greenish brown color, pH 10.5 (11 is better than 10). When green soap is started to form, it means that you've added far too much HCl. MDMA free base will settle on a reaction vessel bottom. Organic layer is drained out (separated).

DCM 200 mL is added to the reaction vessel with water layer and the mixture is stirred for 10 min. The stirrer is stopped and reaction mixture is left 30 min. DCM with the rest MDMA freebase will settle on the vessel bottom. Organic layer is drained out and extracts are combined. There is ~1750 mL of MDMA free base and DCM.

Notes: You can basify the water layer again with conc. NaOH solution to pH 13-14 and drain out MDMA free base residue again.


Purification
A vacuum distillation setup is prepared. Methanol, DCM, water and other low boiling substances are distilled off at 130 °C firstly. Then, a heater is set at 165 °C, little drops of MDMA oil are condensated and seen around 140-145 °C; at 160-165 °C (20-18 mbar) MDMA oil is distilled intensively. The clean MDMA free base distillation yield is ~ 1.0 L.

A membrane vacuum aspirator is sufficient to distill off water, methanol and other low boiling substances from the reaction mixture. A decent vacuum pump is recommended to distill MDMA free base.
Crystallization
MDMA free base is mixed with clean, cold (-10 to -20 C), dry acetone 1:4, dry HCl gas is bubbled through this solution to reach pH 7-6.5. It have to be done carefully. A thick, white crystal mass will be formed after ~5 min bubbling. pH Have to be checked frequently with pH-meter or indicator paper. If the solution become hot, place it into a big freezer to cool it down and continue with a next cold batch. Be very careful and don't drop pH below 7 to 6.5 because MDMA*HCl crystals will dissolve again. In this case, you have to add NaOH base solution again until pH rise up to 7. At least 200 mL base have to be kept ready for spare case of mistakes. The acetone/powder mix is filtered and dried on Buchner funnel with aspirator vacuum. Then, MDMA*HCl is dried again on a Pyrex dish under A/C or a slow blowing fan flow in a dry room.
G.PattonCan change methylamine hci to solution?
 

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Win Win

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Do you understand that methylamine gas is used in order to make methylamine methanol (MeOH) solution? Not methylamine hydrochloride methanol solution. You can directly use methylamine free base methanol solution.
G.PattonNoted with thanks
 

alquimista00

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hello, i don't know if i did something wrong but i could only get 700ml of mdma free base, and when i was doing the distillation the oil distilled at 275 c,so i'm not sure if what i distilled mdma oil or another substane. ph 6
 

JustBrowsing223

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hello, i don't know if i did something wrong but i could only get 700ml of mdma free base, and when i was doing the distillation the oil distilled at 275 c,so i'm not sure if what i distilled mdma oil or another substane. ph 6
alquimista00Could it be that you did simple distillation? According to wikipedia BP seems to be close to that.
 

alquimista00

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Hi i got 700ml of mdma freebase. but it destilled at 275c so i'm not sure if what i distilled was mdma oil. the ph is 6 so for crystaliation i need to raise the ph and i would like to know how?? if ou can help me, than you.
 

WillD

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Hi i got 700ml of mdma freebase. but it destilled at 275c so i'm not sure if what i distilled was mdma oil. the ph is 6 so for crystaliation i need to raise the ph and i would like to know how?? if ou can help me, than you.
alquimista00maybe u have unreacted mdp2p or u get -ol variations after mdp2p+NaBH4 react... Alkyl amine variations have a basic pH.
 

JustBrowsing223

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Hey there! Some dummy questions.
Sodium borohydride (NaBH4) 100 g is added in portions, one teaspoon per ~5 min, H2 gas bubbling has to disappear before next addition (wash down with methanol)
What does wash down with methanol mean? Just use methanol to wash powder thats sticked to glassware ?
Temperature is maintain between 8-10 °C. Sodium borohydride (NaBH4) addition is taken 2-7 h. The mixture is stirred for 2 days.
If its stirred for 48h , the temperature needs to be maintained at 8-9 degrees or it can go to room temp?
A decent vacuum pump is recommended to distill MDMA free base.
Whats decent vacuum pump? Sorry, i have no experience with vac. distillation yet.
 

JustBrowsing223

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Hey there! Some dummy questions.

What does wash down with methanol mean? Just use methanol to wash powder thats sticked to glassware ?

If its stirred for 48h , the temperature needs to be maintained at 8-9 degrees or it can go to room temp?

Whats decent vacuum pump? Sorry, i have no experience with vac. distillation yet.
JustBrowsing223@William Dampier @G.Patton Just tagging some experts. :)
 

G.Patton

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Hey there! Some dummy questions.

What does wash down with methanol mean? Just use methanol to wash powder thats sticked to glassware ?

If its stirred for 48h , the temperature needs to be maintained at 8-9 degrees or it can go to room temp?

Whats decent vacuum pump? Sorry, i have no experience with vac. distillation yet.
JustBrowsing223Hello. Sorry for a long reply.
What does wash down with methanol mean? Just use methanol to wash powder thats sticked to glassware ?
Yes, it means a rinsing NaBH4 from glassware sides.
If its stirred for 48h , the temperature needs to be maintained at 8-9 degrees or it can go to room temp?
8-9 deg have to be maintained for NaBH4 addition. 48h at room temp, correct.
Whats decent vacuum pump? Sorry, i have no experience with vac. distillation yet.
A vacuum pump, which is able to make 0.2-0.4 torr pressure inside distillation apparatus. If you have no experience, I recommend you to learn about distillation. Vacuum distillation apparatus can explode with inappropriate handling. Distillation and distillation systems
Boiling point105 ºC (0.4 torr)
 

spiritveg

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Can I use 39% dimethylamine aqueous solution instead of methylamine gas? If yes then what should be the ratio?
 

Dokodox

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Anybody know if temperatures are highly important or a way to do all in steel so don’t have to import glassware
 

OrgUnikum

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Anybody know if temperatures are highly important or a way to do all in steel so don’t have to import glassware
DokodoxAs long you don't get overboard with any part where the reaction is rendered acidic as in PMK to MDP2P and completely refrain from adding any organic acids SS 316 is fine. Treat the parts with hot 75% H3PO4 for some hours for passivation before the first time using them and thats that.

Keeping temperatures low during the reaction is essential, with big vessels I recommend strongly to have some internal coils installed for cooling additionally to the cooling mantle, and get a powerful industrial chiller. But temp control is much easier in metal then in glass, heat-transfer is better in metal by magnitudes.
 

Dokodox

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As long you don't get overboard with any part where the reaction is rendered acidic as in PMK to MDP2P and completely refrain from adding any organic acids SS 316 is fine. Treat the parts with hot 75% H3PO4 for some hours for passivation before the first time using them and thats that.

Keeping temperatures low during the reaction is essential, with big vessels I recommend strongly to have some internal coils installed for cooling additionally to the cooling mantle, and get a powerful industrial chiller. But temp control is much easier in metal then in glass, heat-transfer is better in metal by magnitudes.
OrgUnikumGona pm you bro
 

clandestinec

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Video in this synthesis would be nice , only ever done PSE reduction through a distiller and through a few solvents , one question on pmk to mdp2p is it HCl powder or on shelf water solution ????
 

malignoalfa

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If I do not extract with DCM (in my country DCM, TOLUENE and XYLENE are highly controlled), how much would be the approximate loss of yield? Thanks for the answer.

Could hexane, benzene, acetone, or ethanol be used for extraction?
 

malignoalfa

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If I do not extract with DCM (in my country DCM, TOLUENE and XYLENE are highly controlled), how much would be the approximate loss of yield? Thanks for the answer.
 
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