G.Patton

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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
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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
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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.
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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.

 
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caesare.robot

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

Hank Schrader

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You can use HCL in any of the solvents. (in isopropanol and others)
You can also use concentrated aqueous acid, dissolve the base in methanol and neutralize with hydrochloric acid and simply put it in the freezer, then you have to wait longer and not the whole crystal will fall out because the mass contains water (In general, it is acceptable).
There is an alternative to hydrochloric acid and this is trimethylchlorosilane and other options.
 

Hank Schrader

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Have you ever seen MDMA trimethylchlorosilane adduct?
G.PattonBy dissolving the amine base in ether... and dissolving trimethylchlorosilane in ether and slowly adding until neutral will give you MDMA chloride. Trimethylchloromilane does not make any adduct, only chloride.
It is a legal replacement for hydrogen chlorine and is very convenient.
 

G.Patton

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By dissolving the amine base in ether... and dissolving trimethylchlorosilane in ether and slowly adding until neutral will give you MDMA chloride. Trimethylchloromilane does not make any adduct, only chloride.
It is a legal replacement for hydrogen chlorine and is very convenient.
Hank SchraderThanks for explanation, I haven't heard about this approach.
 

Zarder

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What type of yields can be expected from this procedure?
 

chuckmcgill

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@G.Patton Hi thanks for your work! Do you have any advice on dissolving the MDMA freebase into DCM? Ours formed an apple sauce in the dcm (it tests purple black in marque reagant). We had dessicant in the mixture (mag sulfate) and used @btcboss2022 invitro methylamine HCL method but our organic layer is not homogenous so we are wondering if there are tricks thanks!
 

G.Patton

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@G.Patton Hi thanks for your work! Do you have any advice on dissolving the MDMA freebase into DCM? Ours formed an apple sauce in the dcm (it tests purple black in marque reagant). We had dessicant in the mixture (mag sulfate) and used @btcboss2022 invitro methylamine HCL method but our organic layer is not homogenous so we are wondering if there are tricks thanks!
chuckmcgill>>>Do you have any advice on dissolving the MDMA freebase into DCM?
What is a problem with dissolving?
>>>We had dessicant in the mixture (mag sulfate)
Have you tried suction filtration? :unsure:
 
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chuckmcgill

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>>>Do you have any advice on dissolving the MDMA freebase into DCM?
What is a problem with dissolving?
>>>We had dessicant in the mixture (mag sulfate)
Have you tried suction filtration? :unsure:
G.PattonThe freebase seems to have formed a massive emulsion layer that sits under the water layer and above the DCM. The layer has the consistency of apple sauce. It tests with marquie as being heavily purple/black and I was able to clean up a little of it through very tedius processing and got a few grams of oil, upon gassing that with hcl got a good yield of nice crystals which passed qualitative testing. Im thinking maybe somehow the desicant (mag sulfate) or other reaction ingredients formed some sort of goop that isnt soluble in DCM but still contains tons of freebase.

Will try vac assist filtration today, its very hard to even get out of the reactor because of how thick it is. Was expecting it to be disolved in DCM not seperate.

Really appreciate the advice thank you so much!
 

G.Patton

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The freebase seems to have formed a massive emulsion layer that sits under the water layer and above the DCM. The layer has the consistency of apple sauce. It tests with marquie as being heavily purple/black and I was able to clean up a little of it through very tedius processing and got a few grams of oil, upon gassing that with hcl got a good yield of nice crystals which passed qualitative testing. Im thinking maybe somehow the desicant (mag sulfate) or other reaction ingredients formed some sort of goop that isnt soluble in DCM but still contains tons of freebase.

Will try vac assist filtration today, its very hard to even get out of the reactor because of how thick it is. Was expecting it to be disolved in DCM not seperate.

Really appreciate the advice thank you so much!
chuckmcgill>>>The freebase seems to have formed a massive emulsion layer that sits under the water layer and above the DCM. The layer has the consistency of apple sauce.
Actually I still don't understand well how it is possible =) Do you have a picture? You had to collect all water by MgSO4 anhydr. or Na2SO4.
 

chuckmcgill

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>>>The freebase seems to have formed a massive emulsion layer that sits under the water layer and above the DCM. The layer has the consistency of apple sauce.
Actually I still don't understand well how it is possible =) Do you have a picture? You had to collect all water by MgSO4 anhydr. or Na2SO4.
G.PattonThanks, Im finding a lot of information online about mgSO4 being used as a water/oil emulsion stabilizer. I did not find this property reported for Na2SO4. I will try Sodium next time and see if I have better results, if not ill get a pic.
 

mygodson

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Thanks, Im finding a lot of information online about mgSO4 being used as a water/oil emulsion stabilizer. I did not find this property reported for Na2SO4. I will try Sodium next time and see if I have better results, if not ill get a pic.
chuckmcgill
Both magnesium sulfate and sodium sulfate can be used, but the sodium sulfate crystal is relatively large and easy to deposit at the bottom, which is good
 

2-79-790125

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@G.Patton Hi thanks for your work! Do you have any advice on dissolving the MDMA freebase into DCM? Ours formed an apple sauce in the dcm (it tests purple black in marque reagant). We had dessicant in the mixture (mag sulfate) and used @btcboss2022 invitro methylamine HCL method but our organic layer is not homogenous so we are wondering if there are tricks thanks!
chuckmcgillsaw you had an emulsion......looking for some tips:
Hi, I need help! : )

  • Benzoquinone Wacker Oxidation of Safrole in Methanol to yield MDP2P
  • From Erowid.org/archive/rhodium/chemistry/wacker.benzo-meoh.html
  • By Methyl Man
Stuck on 5% NaOH Wash #2. Wash #1 was as expected, resulting in a very black top “aqueous?” layer that was discarded. When washing the bottom layer that presumably contains DCM and the Ketone with a 2nd 5% NaOH a massive amount of, I think, hydroquinone appeared. I drained the bottom layer to wash a third time, kept the top layer from 5%NaOH wash #2 just in case, and washed all the hydroquinone easily from the sep funnel. After adding the 3rd 5% NaOH Wash, I have a muddy green emulsion with zero separation.

Questions: Why didn’t the hydroquinone appear in the 1st wash?

Are my instructions 100% accurate that the top layer from the 1st 5%NaOH wash was “Aqueous” and therefore did NOT contain the Ketone and could be discarded? Or did I just throw away all my hard work and money?

Why does the emulsion seem to be getting worse with each NaOH wash instead of better?

What’s the best way to break up this emulsion?

Thanks. Its frustrating. Everything was going well up to this point.
 

Zarder

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It sounds to me like your dessicant has formed a kind of mud with the freebase in the bottom of your reactor.
I’m wondering if a dessicant is even necessary
 

G.Patton

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It sounds to me like your dessicant has formed a kind of mud with the freebase in the bottom of your reactor.
I’m wondering if a dessicant is even necessary
ZarderIt have to be use in pair with solvent. In opposite case your oil will be remained on desiccant.
 

StarWars

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