MDMA synthesis via NaBH4 from MDP2P

[bitcoinup2020]

Please help explain more information in this section.
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.

After adding all the sodium borohydride (NaBH4), we can reduce the stirring time to 4 hours right now, can I do the next step? or must complete 48 hours

Thank you very much for the answer.

 

[G.Patton]

Please help explain more information in this section.
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.

After adding all the sodium borohydride (NaBH4), we can reduce the stirring time to 4 hours right now, can I do the next step? or must complete 48 hours

Thank you very much for the answer.

bitcoinup2020Hello. There is clearly written that yes, you can. You will lose about 10-20% yield.

 

[bblanco]

Hello. There is clearly written that yes, you can. You will lose about 10-20% yield.

G.Pattoni scaled it to 10gr mdp2p.. haha if you know how i, as 6 week old suburban sjamaan worked to something which i made following these steps but only as 1234... i did not use stirrer, vaccum pump jadaa. in the 6 weeks destroyed my 2 bigggest rbf and when needed sep. funnel BAM ... no funnel for me anymore...
did not waited like mentioned just stirred and put some swung in it in ended up with as i would describe described kind of mdma... its a start but i want to see crystals... but.. most talk here is theoraticly... im different... as i had to know if mdma, filled a capsule like 13-14 h ago... under 200mg.. look it misses 2 aspects which i remember MDMA which i describe the yawning folllowed by the tunnel flows over in a x amounts of hours pink sunglasses vibe and just love...
that was 10 years ago.. now no yawning no real tunnel... for the rest i think higher dose and i would be 100% but at least it fucking sweet..

 

[JESSIE]

can you directly use methalymine 40% in methanol instead of disolving the gas ( should you handle other ratio)

 

[G.Patton]

can you directly use methalymine 40% in methanol instead of disolving the gas ( should you handle other ratio)

JESSIEHello, yes, you can.

 

[JESSIE]

Hello, yes, you can.

G.Pattonthanks for the contribution

 

[rothschild33]

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

View attachment 8287 ​

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.​

View attachment 8288 ​

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.Patton

I might be missing something but at 'MDP2P reduction to MDMA', wouldn't adding HCl lower the pH level? if the pH level does go low, should it be countered with adding more NaOH?

 

[G.Patton]

I might be missing something but at 'MDP2P reduction to MDMA', wouldn't adding HCl lower the pH level? if the pH level does go low, should it be countered with adding more NaOH?

rothschild33Hello, which HCl addition step do you mean? There is correct manual.

 

[rothschild33]

Hello, which HCl addition step do you mean? There is correct manual.

G.Patton

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)

 

[G.Patton]

You don't need to change any. pH is lowered in the water layer, which will be extracted and than discarded

 

[Wendy]

Why do we have to partially neutralize free base after imine reduction?

 

[G.Patton]

Why do we have to partially neutralize free base after imine reduction?

WendyDo you mean the acid addition? It allow us to get rid of sodium borohydride excess after reaction.

 

[bitcoinup2020]

Can we dissolve 300g of Methylamine HCL (10%) in 3000 g of Methanol and then add NaOH to convert Methylamine HCL to Methylamine Freebase instead of compressing 300g of Methylamine gas (10%) in 3000 g of Methanol? If yes, how many NaOH should we use gram?

Thank you very much for the answer.

 

[G.Patton]

Can we dissolve 300g of Methylamine HCL (10%) in 3000 g of Methanol and then add NaOH to convert Methylamine HCL to Methylamine Freebase instead of compressing 300g of Methylamine gas (10%) in 3000 g of Methanol? If yes, how many NaOH should we use gram?

Thank you very much for the answer.

bitcoinup2020You can dissolve 300 g methylamine free base by any convenient for you way. 300 g of Methylamine*HCl contain about half of hydrochloric acid. Hence, if you make your manipulation with Methylamine HCl in MeOH solution, you'll get at least half of necessary quantity of methylamine free base.

P.S. Please, read and learn Moles, grams, litres and chemical calculations in Laboratory FAQ section and count it by yourself.

 

[bitcoinup2020]

You can dissolve 300 g methylamine free base by any convenient for you way. 300 g of Methylamine*HCl contain about half of hydrochloric acid. Hence, if you make your manipulation with Methylamine HCl in MeOH solution, you'll get at least half of necessary quantity of methylamine free base.

P.S. Please, read and learn Moles, grams, litres and chemical calculations in Laboratory FAQ section and count it by yourself.

G.PattonThank you very much for the answer.

I will learn more skills https://bbgate.com/threads/moles-grams-litres-and-chemical-calculations.5295/

I love BB

 

[Stretcher5335]

Can this be used as a starting material

 

[rothschild33]

Can this be used as a starting material

View attachment 12641​

Stretcher5335what's the CAS?

 

[Stretcher5335]

CAS # 1205-17-0
3-(1,3-Benzodioxol-5-yl)-2-Methylpropanal

 

[workworkwork]

What type of overhead stirrer is acceptable for this reaction?
I bought a cheap one from Aliexpress sold by Vevor. And I bought a second one more powerful with 200w. Now I'm afraid that stirrers are dangerous for this reaction. I will be adding borohydride 5 in 5 minutes and there will be hydrogen production that is an explosive gas.
I learned there is 2 types of stirrers, brushed and brushless, maybe because of that some cost 200 euros and others cost 800. Do I have buy a 800 euros stirrer?

 

[AKWA]

What type of overhead stirrer is acceptable for this reaction?
I bought a cheap one from Aliexpress sold by Vevor. And I bought a second one more powerful with 200w. Now I'm afraid that stirrers are dangerous for this reaction. I will be adding borohydride 5 in 5 minutes and there will be hydrogen production that is an explosive gas.
I learned there is 2 types of stirrers, brushed and brushless, maybe because of that some cost 200 euros and others cost 800. Do I have buy a 800 euros stirrer?

workworkworkWhy do you think overhead stirrers are dangerous for this reaction?

 

[workworkwork]

I bought 2 cheap stirrers from aliexpress. I was thinking they were good to start. But the difference between a 200 euros stirrer and a 800 is not only the durability as I was thinking. Maybe the cheap ones I bough from aliexpress are not suitable for this reaction and I will need buy a 800 euros stirrer from a good brand. Not sure if the cheap one make sparks and if sparks is a problem or not in this reaction, if the H2 production is enough to make an explosion. Or another problem I'm not thinking yet.

 

[Studenttt]

I have 40% Methylamine in Methanol Solution, can i put 750 ml for 1 liter of pmk?

 

[workworkwork]

This?
Methylamine (40% in Methanol, ca. 9.8mol/L)
9.8 mol x 31g = 304g, so exactly 1L solution per 1L MDP2P

 

[Studenttt]

Okay thank you verry much,
so i can just put 1 Liter methylamine 40% in methanol on 1 liter mdp2p is not needed to put extra 2 liter methanol on it?

 

[bmkadbbsupplier]

Okay thank you verry much,
so i can just put 1 Liter methylamine 40% in methanol on 1 liter mdp2p is not needed to put extra 2 liter methanol on it?

Studentttyes