MDMA synthesis via Pt/H2. Small scale.

[WillD]

Reaction scheme:

​

Reagents:​

• Methylamine 40% aq (cas 74-89-5) 2 ml;​
• Ethanol (EtOH) 5 ml;​
• 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; PMK; cas 4676-39-5) 2 ml;​
• Adams' catalyst (PtO2; cas 1314-15-4) 0.05 g;​
• Distilled water 165 ml;​
• Hydrochloric acid (36% aq HCl);​
• Dichloromethane 450 ml;​
• Dodium hydroxide solution (25% aq NaOH);​
• MgSO4 anhydrous;​
• Isopropyl alcohol (IPA) ~50 ml;​
• Diethyl ether ~50 ml;​

Equipment and glassware:

​

• Pear shaped flask 10 ml;​
• Retort stand and clamp for securing apparatus (optional);​
• Hydrogen gas (H2) source;​
• Vessel for height pressure reaction with manometer (thick glass champagne bottle can be modified for this synthesis);​
• Hoses;​
• Syringe or Pasteur pipette;​
• pH indicator papers;​
• Beakers (50 mL x2, 100 mL x2);​
• Vacuum source;​
• Laboratory scale (0.1-200 g is suitable);​
• Measuring cylinder 10 mL;​
• Glass rod and spatula;​
• Separatory funnel 0.5 L (optional);​
• Buchner flask and Schott funnel; ​
• Vacuum in desiccator (optional);​
• Rotary evaporator (optional);​

Synthesis:

1. Methylamine 40% aq 2 ml is added to ethanol (EtOH) 5 ml.
2. 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; PMK) 2 ml is slowly poured into the mixture and stirred for 1 h at room temperature.
3. Adams' catalyst (PtO2) 0.05 g is added to the mixture under nitrogen flow.
4. Reaction mixture is placed under a hydrogen atmosphere at 56 psi (3.86 bar) for 3.5 h.
5. The pressure have to be returned to 56 psi at the 1 and 2 h of exposure in the vessel.
6. A reek and PtO2 is removed in vacuum after filtration through Celite with ethanol.
7. The residue is dissolved in distilled water 165 ml and acidified with hydrochloric acid (36% aq HCl) to pH 1. Then, extracted with DCM (3x75 ml).
8. The aqueous phase is alkalized with sodium hydroxide solution (25% aq NaOH) to pH 10 and organic substances are extracted with DCM (3x75 ml).
9. Additional sodium hydroxide solution (NaOH aq 25%) 10 and 20 drops are added before the second and third DCM extractions respectively.
10. Combined organic layers are dried over MgSO4 anhydrous and concentrated in vacuum to give clean amber MDMA free base oil. The yield is 2.0 g (~76 %).
11. MDMA free base oil 2 g is dissolved in isopropyl alcohol (IPA) 3.5 ml and acidified with hydrochloric acid (HCl aq 36 %) ~40 drops to reach pH 5.5-6.
12. The solvent is removed under vacuum with heat, a precipitate is formed (color range from white to pink and to brown). The precipitate of MDMA hydrochloride is homogenized and washed with a IPA:ether 2:1 solution before a final washing with ether on Buchner flask and Schott funnel.
13. The resulting white MDMA hydrochloride is dried under vacuum in desiccator. The yield is 2.3 g (total yield ~73 %).​

 

[merlin]

Reaction scheme:
View attachment 1307

Synthesis:
1. To ethanol (5 ml) was added a solution of 40% methylamine in water (2 ml).
2. PMK (2 ml) was slowly added to the mixture and allowed to stir at room temperature for 1 h.
3. To the mixture was added PtO2 (0.05 g) under a stream of nitrogen.
4. The resultant mixture was placed under a hydrogen atmosphere at 56 psi for 3.5 h.
5. The pressure in the device was returned to 56 psi at the 1 and 2 h marks.
6. After filtration through celite with ethanol to remove PtO2, the reek were removed in vacuum.
7. The residue was dissolved in water (165 ml) and acidified with 32% aqueous HCl (pH=1) and extracted with DCM (3x75 ml).
8. The aqueous phase was basified with 25% aqueous NaOH (pH=10) and the organics extracted with DCM (3x75 ml).
9. A further 10 and 20 drops of 25% aqueous NaOH were added before the second and third DCM extractions, respectively.
10. The combined organic layers were dried over MgSO4 and concentrated to give clean MDMA as an amber oil (2.0 g yield).
11. Dissolving the base (2 g) in isopropyl alcohol (3.5 ml) and acidifying with 37% aqueous HCl (40 drops).
12. The solvent was removed in vacuum with heat to reveal a precipitate (ranging in color from white to pink to brown) which was homogenized and washed with a 2:1 isopropyl alcohol:ether solution before a final wash with ether.
13. The resulting white MDMA hydrochloride was dried under high vacuum(yield 2.3 g).

William Dampier

​

Synthesis:
1. To ethanol (5 ml) was added a solution of 40% methylamine in water (2 ml).
2. PMK (2 ml) was slowly added to the mixture and allowed to stir at room temperature for 1 h.
3. To the mixture was added PtO2 (0.05 g) under a stream of nitrogen.

what is pt02?????
4. The resultant mixture was placed under a hydrogen atmosphere at 56 psi for 3.5 h.
5. The pressure in the device was returned to 56 psi at the 1 and 2 h marks.

What tool are you using ? what are they putting the hydrogen into ?

6. After filtration through celite with ethanol to remove PtO2, the reek were removed in vacuum. p
7. The residue was dissolved in water (165 ml) and acidified with 32% aqueous HCl (pH=1) and extracted with DCM (3x75 ml). DCM what is that ?
8. The aqueous phase was basified with 25% aqueous NaOH (pH=10) and the organics extracted with DCM (3x75 ml).
9. A further 10 and 20 drops of 25% aqueous NaOH were added before the second and third DCM extractions, respectively.
10. The combined organic layers were dried over MgSO4 and concentrated to give clean MDMA as an amber oil (2.0 g yield). ( why is dry over)
11. Dissolving the base (2 g) in isopropyl alcohol (3.5 ml) and acidifying with 37% aqueous HCl (40 drops).
12. The solvent was removed in vacuum with heat to reveal a precipitate (ranging in color from white to pink to brown) which was homogenized and washed with a 2:1 isopropyl alcohol:ether solution before a final wash with ether.
13. The resulting white MDMA hydrochloride was dried under high vacuum(yield 2.3 g).

 

[MadHatter]

what is pt02?????
DCM what is that ?

merlinPlease.

https://gprivate.com/612xd

 

[merlin]

that was pretty cool

Please.

https://gprivate.com/612xd

DocXhar

 

[workworkwork]

Amazing yield!
Possible do this reaction for bigger quantities?
DCM can be reused?

 

[KokosDreams]

Amazing addition to the forum!

Will you guys add hydrogenation synthesis routes for amphetamine aswell?

 

[MadHatter]

4. The resultant mixture was placed under a hydrogen atmosphere at 56 psi for 3.5 h.
5. The pressure in the device was returned to 56 psi at the 1 and 2 h marks.

William DampierSorry, I don't fully understand these two sentences? Is there something wrong there? We start at 56 psi and then ... return to 56 psi?

Also, what kind of device is adviceable for this kind of pressurized reaction? 56 psi is quite a bit of pressure, given that the normal tire pressure lies in the 30:ish-range. Normal glassware won't cut it, right?

 

[G.Patton]

Sorry, I don't fully understand these two sentences? Is there something wrong there? We start at 56 psi and then ... return to 56 psi?

Also, what kind of device is adviceable for this kind of pressurized reaction? 56 psi is quite a bit of pressure, given that the normal tire pressure lies in the 30:ish-range. Normal glassware won't cut it, right?

DocXHi, sorry for a long reply. The pressure during reaction can be changed because hydrogen is used for reduction. You have to pump H2 to this pressure after 1 and 2 h of reaction. I thing in this small scale it isn't significant. You have to use steel reactor or thick glass for high pressure. I added picture with a tip.

 

[MadHatter]

Hi, sorry for a long reply. The pressure during reaction can be changed because hydrogen is used for reduction. You have to pump H2 to this pressure after 1 and 2 h of reaction. I thing in this small scale it isn't significant. You have to use steel reactor or thick glass for high pressure. I added picture with a tip.

G.PattonGreat tip with the champagne bottle!

So it isn't a constant pressure of 56 psi for 3,5 hours? Sorry, I still don't fully understand. I read nr 4 as "pump H2 into the vessel with the reactants to a pressure of 56 psi. Keep it there for 3.5 hours"
which makes nr 5 a bit strange. Should we lower the pressure and then pump it up to 56 psi again at 1 and 2 hours?

 

[G.Patton]

So it isn't a constant pressure of 56 psi for 3,5 hours?

DocXNo, you have to keep 56 psi during reaction. Just chek it on 2 and 3h of reaction.

 

[MadHatter]

No, you have to keep 56 psi during reaction. Just chek it on 2 and 3h of reaction.

G.PattonD'accord. Then I understand.

 

[Katty Korner]

Maybe I missed it on the forums, but a guide to making a steel reactor for such hydrogenations would be a huge help to all.

Afaik precious metal catalyst hydrogenations are how the big dogs do it in the Netherlands. Read how maybe 10 or less years back police over there found a trailer full of reagents and what not, and many canisters of hydrogen were found

 

[Davidrobinson]

Has this synth been tested out. Can you tell me how the imine is 100% formed with water present.

 

[Katty Korner]

Has this synth been tested out. Can you tell me how the imine is 100% formed with water present.

oscar412I can't find the paper, but it's somewhere over at the vespiary. There was a route invented of using benzodioxole and a grignard I think, it was basically just saying here is how it could be made if it was legal.

In this they happily formed the imine in water, so I think if you trawl the "drugs and syntheis" forum, you'll find it.

 

[dirktem]

Reaction scheme:

View attachment 7151 ​

Reagents:​

• Methylamine 40% aq (cas 74-89-5) 2 ml;​
• Ethanol (EtOH) 5 ml;​
• 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; PMK; cas 4676-39-5) 2 ml;​
• Adams' catalyst (PtO2; cas 1314-15-4) 0.05 g;​
• Distilled water 165 ml;​
• Hydrochloric acid (36% aq HCl);​
• Dichloromethane 450 ml;​
• Dodium hydroxide solution (25% aq NaOH);​
• MgSO4 anhydrous;​
• Isopropyl alcohol (IPA) ~50 ml;​
• Diethyl ether ~50 ml;​

Equipment and glassware: View attachment 7152 ​

• Pear shaped flask 10 ml;​
• Retort stand and clamp for securing apparatus (optional);​
• Hydrogen gas (H2) source;​
• Vessel for height pressure reaction with manometer (thick glass champagne bottle can be modified for this synthesis);​
• Hoses;​
• Syringe or Pasteur pipette;​
• pH indicator papers;​
• Beakers (50 mL x2, 100 mL x2);​
• Vacuum source;​
• Laboratory scale (0.1-200 g is suitable);​
• Measuring cylinder 10 mL;​
• Glass rod and spatula;​
• Separatory funnel 0.5 L (optional);​
• Buchner flask and Schott funnel; ​
• Vacuum in desiccator (optional);​
• Rotary evaporator (optional);​

Synthesis:

1. Methylamine 40% aq 2 ml is added to ethanol (EtOH) 5 ml.
2. 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; PMK) 2 ml is slowly poured into the mixture and stirred for 1 h at room temperature.
3. Adams' catalyst (PtO2) 0.05 g is added to the mixture under nitrogen flow.
4. Reaction mixture is placed under a hydrogen atmosphere at 56 psi (3.86 bar) for 3.5 h.
5. The pressure have to be returned to 56 psi at the 1 and 2 h of exposure in the vessel.
6. A reek and PtO2 is removed in vacuum after filtration through Celite with ethanol.
7. The residue is dissolved in distilled water 165 ml and acidified with hydrochloric acid (36% aq HCl) to pH 1. Then, extracted with DCM (3x75 ml).
8. The aqueous phase is alkalized with sodium hydroxide solution (25% aq NaOH) to pH 10 and organic substances are extracted with DCM (3x75 ml).
9. Additional sodium hydroxide solution (NaOH aq 25%) 10 and 20 drops are added before the second and third DCM extractions respectively.
10. Combined organic layers are dried over MgSO4 anhydrous and concentrated in vacuum to give clean amber MDMA free base oil. The yield is 2.0 g (~76 %).
11. MDMA free base oil 2 g is dissolved in isopropyl alcohol (IPA) 3.5 ml and acidified with hydrochloric acid (HCl aq 36 %) ~40 drops to reach pH 5.5-6.
12. The solvent is removed under vacuum with heat, a precipitate is formed (color range from white to pink and to brown). The precipitate of MDMA hydrochloride is homogenized and washed with a IPA:ether 2:1 solution before a final washing with ether on Buchner flask and Schott funnel.
13. The resulting white MDMA hydrochloride is dried under vacuum in desiccator. The yield is 2.3 g (total yield ~73 %).​

William DampierYou all are pro, hope to stay and learn

 

[dirktem]

I have no chem backround