( the prefixes "Methcathinone" or "Methylone" or "βk-MDMA" were not available so I had to put "MDMA" but it's not the synthesis of MDMA that is presented here but that of methylone which is the beta-ketone version of MDMA )
Ingredients:
20g of 3,4-Methylenedioxypropiophenone (=MDP1P) (CAS 28281-49-4)
90ml dichloromethane (=DCM)
22g bromine
50ml sodium thiosulfate 10%
50ml n-Methylpyrrolidone
20ml methylamine 40%
30g magnesium sulfate
10ml hydrochloric acid
Sodium bicarbonate solution (12g in 120ml)
Distilled water
Acetone
Equipment:
250ml round-bottomed flask (+stand)
Magnetic stirrer
Syringe / pipette
pH paper
Beakers
Balance
Ice bath
Stirring supplies
Thermometer
Filter
Optional :
Condenser
Separating funnel
Procedure:
1: 20g of MDP1P are dissolved in 60ml of DCM, then a few drops of hydrochloric acid and 22g of boron (drop by drop) follow
-> The reaction is exothermic
2 : Afterwards, the remaining boron is removed with 10% sodium thiosulfate solution and the solution is washed with distilled water
The organic layer ( 2-Bromo-3,4-methylenedioxypropiophenone) is recovered for the next step (it can also be distilled under vacuum to obtain a solid).
3: The recovered organic layer is dissolved in 50ml of n-methylpyrrolidone and 20ml of 40% methylamine is added, then the flask is sealed and shaken
-> The reaction is exothermic and must be controlled (if the pressure is too high, the flask is placed in an ice bath to keep the temperature below 55ºC).
4: The solution is then washed with sodium bicarbonate and stirred for one or two minutes.
5: 30ml of DCM are added with stirring for 5min, then the free methylone base is extracted (organic layer, bottom layer)
The inorganic layer may still contain the desired substance, so step 5 can be repeated once again.
6: The organic layers obtained are combined and washed 3-4 times with 60ml of distilled water until the smell of methylamine can no longer be detected; the bottom layer is recovered and dried over magnesium sulfate.
7: Our volume of free base is diluted with the same volume of acetone and then dropwise treated with hydrochloric acid to obtain a pH of 5.5 - 6 (if the solution becomes thick, acetone is added).
8: The whole is filtered to obtain our long-awaited βk-MDMA. However, our product is not pure, so it can be washed with acetone
Before purification:
After purification:
9: If crystallization is desired, add 1.5ml of distilled water and 1ml of acetone to each gram of methylone HCl, and allow to crystallize as for 4MMC.
Ingredients:
20g of 3,4-Methylenedioxypropiophenone (=MDP1P) (CAS 28281-49-4)
90ml dichloromethane (=DCM)
22g bromine
50ml sodium thiosulfate 10%
50ml n-Methylpyrrolidone
20ml methylamine 40%
30g magnesium sulfate
10ml hydrochloric acid
Sodium bicarbonate solution (12g in 120ml)
Distilled water
Acetone
Equipment:
250ml round-bottomed flask (+stand)
Magnetic stirrer
Syringe / pipette
pH paper
Beakers
Balance
Ice bath
Stirring supplies
Thermometer
Filter
Optional :
Condenser
Separating funnel
Procedure:
1: 20g of MDP1P are dissolved in 60ml of DCM, then a few drops of hydrochloric acid and 22g of boron (drop by drop) follow
-> The reaction is exothermic
2 : Afterwards, the remaining boron is removed with 10% sodium thiosulfate solution and the solution is washed with distilled water
The organic layer ( 2-Bromo-3,4-methylenedioxypropiophenone) is recovered for the next step (it can also be distilled under vacuum to obtain a solid).
3: The recovered organic layer is dissolved in 50ml of n-methylpyrrolidone and 20ml of 40% methylamine is added, then the flask is sealed and shaken
-> The reaction is exothermic and must be controlled (if the pressure is too high, the flask is placed in an ice bath to keep the temperature below 55ºC).
4: The solution is then washed with sodium bicarbonate and stirred for one or two minutes.
5: 30ml of DCM are added with stirring for 5min, then the free methylone base is extracted (organic layer, bottom layer)
The inorganic layer may still contain the desired substance, so step 5 can be repeated once again.
6: The organic layers obtained are combined and washed 3-4 times with 60ml of distilled water until the smell of methylamine can no longer be detected; the bottom layer is recovered and dried over magnesium sulfate.
7: Our volume of free base is diluted with the same volume of acetone and then dropwise treated with hydrochloric acid to obtain a pH of 5.5 - 6 (if the solution becomes thick, acetone is added).
8: The whole is filtered to obtain our long-awaited βk-MDMA. However, our product is not pure, so it can be washed with acetone
Before purification:
After purification:
9: If crystallization is desired, add 1.5ml of distilled water and 1ml of acetone to each gram of methylone HCl, and allow to crystallize as for 4MMC.
