MDMA synthesis via NaBH4 from 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

 

[Studenttt]

Is this synthese possible white methylamine 40% in water?

 

[mr.j499]

is it necessary to use methlylamine gas?can it be replaced with methanol soution?

 

[bmkadbbsupplier]

is it necessary to use methlylamine gas?can it be replaced with methanol soution?

mr.j499Methylamine solution can be used.methylamine solution can be used instead of methanol solution

 

[mr.j499]

Methylamine solution can be used.methylamine solution can be used instead of methanol solution

bmkadbbsupplierif its water solution of methylamine same?

 

[artificialmango]

@G.Patton Hey I ran this reaction exactly as written out in this procedure and everything happened as it should up to the point where the post-reaction work up began, and that's where I would like some further clarity if possible.

After 36 hours of stirring at RT following the addition of 100g borohydride, 8L of H20 with 8ml 37% HCL acid were added to the reaction mixture to quench any remaining borohydride with stirring.
Following 10 mins of stirring and 20 mins to settle, (pH was 10) a dark brown freebase formed a bottom layer and was separated from the aqueous layer on top. The aqueous layer remaining in the flask was extracted with 200ml DCM twice, then the combined organic extracts were pooled together.
The aqueous layer was then further basified to pH14 with 30% NaOH solution and allowed to settle. A thin layer of what looked to be freebase oil began to form on top of the water layer, unfortunately after attempting to extract the remaining freebase with another 200ml of DCM, this formed an emulsion that couldnt be broken up and was forced to throw out.

This left roughly 700ml of freebase + DCM (dark brownish red pH is basic for sure). From this point forward, the DCM was rotovapped off and the methanol. (I am thinking this is where the fuck up occurred, should have dried over mgso4 first before evaporating the solvents).

The concentrate was collected and 100g was separated from the main batch of base and dissolved in roughly 4x its volume in chilled IPA (pH was 9) and then gassed with hcl until solution was pH7 but no crystals formed in the solution. The gassed IPA/freebase was put in the freezer along with the main batch of base that remains ungassed.

Where did I go wrong and what can I do to imprve my work up and possibly make my freebase oil a little lighter in colour (any suggestions for washes at certain points in the work up, if so what sort and what order should they be done in). Any idea why crystals did not form when gassed with HCl Gas in the small 100g amount of freebase I trialed this work up with? Any help would be appreciated.

 

[G.Patton]

@G.Patton Hey I ran this reaction exactly as written out in this procedure and everything happened as it should up to the point where the post-reaction work up began, and that's where I would like some further clarity if possible.

After 36 hours of stirring at RT following the addition of 100g borohydride, 8L of H20 with 8ml 37% HCL acid were added to the reaction mixture to quench any remaining borohydride with stirring.
Following 10 mins of stirring and 20 mins to settle, (pH was 10) a dark brown freebase formed a bottom layer and was separated from the aqueous layer on top. The aqueous layer remaining in the flask was extracted with 200ml DCM twice, then the combined organic extracts were pooled together.
The aqueous layer was then further basified to pH14 with 30% NaOH solution and allowed to settle. A thin layer of what looked to be freebase oil began to form on top of the water layer, unfortunately after attempting to extract the remaining freebase with another 200ml of DCM, this formed an emulsion that couldnt be broken up and was forced to throw out.

This left roughly 700ml of freebase + DCM (dark brownish red pH is basic for sure). From this point forward, the DCM was rotovapped off and the methanol. (I am thinking this is where the fuck up occurred, should have dried over mgso4 first before evaporating the solvents).

The concentrate was collected and 100g was separated from the main batch of base and dissolved in roughly 4x its volume in chilled IPA (pH was 9) and then gassed with hcl until solution was pH7 but no crystals formed in the solution. The gassed IPA/freebase was put in the freezer along with the main batch of base that remains ungassed.

Where did I go wrong and what can I do to imprve my work up and possibly make my freebase oil a little lighter in colour (any suggestions for washes at certain points in the work up, if so what sort and what order should they be done in). Any idea why crystals did not form when gassed with HCl Gas in the small 100g amount of freebase I trialed this work up with? Any help would be appreciated.

artificialmango

unfortunately after attempting to extract the remaining freebase with another 200ml of DCM, this formed an emulsion that couldnt be broken up and was forced to throw out.

Hello, Have you tried to add NaCl or use an ultrasonic?

(I am thinking this is where the fuck up occurred, should have dried over mgso4 first before evaporating the solvents)

Do u mean dry before the synthesis? I don't understand this statement well, sorry.

The gassed IPA/freebase was put in the freezer

Did you get MDMDA*HCl crystals after freezing? You can rub vessel walls by glass rod to make crystallization centers.

 

[Newbee]

Questions:
I Have 33% Methylamine in methanol solution (which is 330g per liter in my understanding if im correct?)
Can I use it? also in receipt was mentioned that Methylamine 330g was dissolved in 3l not 1l (as 33% in 1l)
Can I just simply pour to my 1l of 33% solution just 2 liters of methanol and mix it? it will be the same as dissolve 330g in 3l?
thanks in advance and sorry if my question might sound stupid for more experienced chemists.

 

[workworkwork]

In the procedure says to dissolve 200ml DCM in about 12L to extract the mdma freebase.
The solubility of DCM in water is 25.6 g/L, means that if I put 200ml DCM in 12L water, no DCM will go to the bottom of the recipient right?
I don't understand, the 200ml DCM will not be lost in the water?

 

[Woodshack]

In the procedure says to dissolve 200ml DCM in about 12L to extract the mdma freebase.
The solubility of DCM in water is 25.6 g/L, means that if I put 200ml DCM in 12L water, no DCM will go to the bottom of the recipient right?
I don't understand, the 200ml DCM will not be lost in the water?

workworkworkDCM is a non-polar solvent, go mix oil and water in your garage as an experiment.

 

[Lordoftheshard 2]

Will this synth work for bmk it should has any one tried making meth with this synth

 

[Calve]

G.Patton Hi, I have some questions.
In the recipe there is hinting of using anhydrous conditions in this manner when methamphetamine is produced from p2p.

"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."

If one would add toluene after the formation of the Schiff Base to create an azeotropic water-toluene mixture wich can be boiled off at 84deg. using a dean-stark trap, wouldn't the reaction be disturbed by that? I guess the unreacted methylamine and methanol would boil off too. How would this be done properly?
Or did it mean substituting the methanol for toluene, but would toluene dissolve the methylamine (wich likes water a lot)?

Won't the formation of the Schiff Base itself, before the nabh4 reduction, be disturbed by the presence of any water?

I hope you have some clarity on this.
Thanks!!

 

[OrgUnikum]

G.Patton Hi, I have some questions.
In the recipe there is hinting of using anhydrous conditions in this manner when methamphetamine is produced from p2p.

"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."

If one would add toluene after the formation of the Schiff Base to create an azeotropic water-toluene mixture wich can be boiled off at 84deg. using a dean-stark trap, wouldn't the reaction be disturbed by that? I guess the unreacted methylamine and methanol would boil off too. How would this be done properly?
Or did it mean substituting the methanol for toluene, but would toluene dissolve the methylamine (wich likes water a lot)?

Won't the formation of the Schiff Base itself, before the nabh4 reduction, be disturbed by the presence of any water?

I hope you have some clarity on this.
Thanks!!

CalveMethylamine is a gas. This makes the idea to remove the water by azeotropic distillation practically impossible.

The best drying agent before a NaBH4 reduction is sodium methoxide.

 

[Jordan Belfort]

G.Patton Hi, I have some questions.
In the recipe there is hinting of using anhydrous conditions in this manner when methamphetamine is produced from p2p.

"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."

If one would add toluene after the formation of the Schiff Base to create an azeotropic water-toluene mixture wich can be boiled off at 84deg. using a dean-stark trap, wouldn't the reaction be disturbed by that? I guess the unreacted methylamine and methanol would boil off too. How would this be done properly?
Or did it mean substituting the methanol for toluene, but would toluene dissolve the methylamine (wich likes water a lot)?

Won't the formation of the Schiff Base itself, before the nabh4 reduction, be disturbed by the presence of any water?

I hope you have some clarity on this.
Thanks!!

CalveUsing hexane is a a better option if the Schiff base is basified over toluene when you use methylamine in methanol.

 

[Woodshack]

What causes the MDMA to turn black? No hcl gas generator was used just Ph'd the freebase oil to ph7 but in the process it dropped abit lower then expected then the Ph was raised back up to 7 using spare freebase. then crashed out with acetone too evap off.

 

[Jordan Belfort]

What causes the MDMA to turn black? No hcl gas generator was used just Ph'd the freebase oil to ph7 but in the process it dropped abit lower then expected then the Ph was raised back up to 7 using spare freebase. then crashed out with acetone too evap off.

WoodshackWhy you don't bubble in tolueen/hexane ? Never Ph issues then

 

[OrgUnikum]

What causes the MDMA to turn black? No hcl gas generator was used just Ph'd the freebase oil to ph7 but in the process it dropped abit lower then expected then the Ph was raised back up to 7 using spare freebase. then crashed out with acetone too evap off.

WoodshackStrongly alkaline conditions in the reaction lead to purple/black product, re-crystallization from IPA/Acetone takes care of this and gives clean product which can be dissolved in water and grown to big crystals again by slow evaporation.
The discoloration are residues from the reaction, probably traces of bor or boride compounds, stuff which simply does not belong in there. You cannot expect to get a consumable product direct from the reaction thats wishthinking nothing else. Some basic workup, steps for purification are always necessary if you want to provide decent quality.

 

[Woodshack]

Strongly alkaline conditions in the reaction lead to purple/black product, re-crystallization from IPA/Acetone takes care of this and gives clean product which can be dissolved in water and grown to big crystals again by slow evaporation.
The discoloration are residues from the reaction, probably traces of bor or boride compounds, stuff which simply does not belong in there. You cannot expect to get a consumable product direct from the reaction thats wishthinking nothing else. Some basic workup, steps for purification are always necessary if you want to provide decent quality.

OrgUnikumOkay thanks so it was the strong Alkaline conditions, your advice was very solid thank you.

 

[Studenttt]

Can i do this synthese in ethanol,
Can i replace methanol to ethanol?

 

[Jordan Belfort]

Can i do this synthese in ethanol,
Can i replace methanol to ethanol?

StudentttYes you can replace methanol with ethanol.