Methylone (3,4-Methylenedioxymethcathinone, βk-MDMA) is a synthetic substance of the cathinone class that is often compared to MDMA. This product is very popular and causes a strong euphoria and empathy. It acts as a powerful aphrodisiac, the effect of which causes an unrestrained desire to have sex.
This article describes the synthesis of a small amount of methylone. I would like to note that the reaction scales linearly and the proportions of all substances are maintained. Methylone is quite easy to produce in large quantities. Its production does not require sophisticated laboratory equipment. This article describes the technology for producing methylone from halogen ketone (2-bromo-3,4-methylenedioxypropiophenone), which is obtained by standard bromination from 3,4-methylenedioxypropiophenone (3,4-(methylenedioxy)phenyl-1-propanone (MDP1P)).
Reagents:
Reagents:
- 3,4-Methylenedioxypropiophenone (MDP1P; cas 28281-49-4) 20 g;
- Dichloromethane (DСM) 90 ml;
- Bromine (Br2) 22 g;
- Sodium thiosulfate (Na2S2O3) aq solution 10% ~50 ml;
- Distilled water;
- n-Methylpyrrolidone (cas 872-50-4) 50 ml;
- Methylamine aqueous 40% 20 ml;
- Sodium bicarbonate 12 g;
- Magnesium sulphate (MgSO4) ~30 g;
- Hydrochloric acid (~35%) ~10 ml;
- Acetone;
Equipment and glassware:
- Flat bottom flask 250 ml;
- Retort stand and clamp for securing apparatus (optional);
- Magnetic stirrer;
- Reflux condenser (optional);
- Funnel;
- Syringe or Pasteur pipette;
- pH indicator papers;
- Beakers (500 mL x1, 250 mL x2; 100 mL x2);
- Vacuum source;
- Laboratory scale (0.1-200 g is suitable);
- Measuring cylinders 100 mL;
- Cold water bath;
- Glass rod and spatula;
- Separatory funnel 1 L (optional);
- Laboratory grade thermometer;
- Buchner flask and funnel;
- Filter paper;
Synthesis procedures
MDP1P 20 g is dissolved in DСM 60 ml and a few drops of hydrochloric acid are added, then bromine 22 g is added dropwise. The reaction is exothermic, the reaction mixture is become dark, then become light by reason of hydrobromide (white gas) releasing. The remaining bromine is removed with 10% sodium thiosulfate aq solution and reaction mixture is washed with water after the end of this reaction. The organic layer can be used for the methylamination reaction (yield ~140% MDP1P) or distill off DСM under vacuum to a solid.
The synthesis is conducted under normal conditions. 2-Bromo-3,4-methylenedioxypropiophenone 10 g from previous step is dissolved with n-methylpyrrolidone 50 ml in the reaction flask. The mixture is stirred until solids are dissolved.
MDP1P 20 g is dissolved in DСM 60 ml and a few drops of hydrochloric acid are added, then bromine 22 g is added dropwise. The reaction is exothermic, the reaction mixture is become dark, then become light by reason of hydrobromide (white gas) releasing. The remaining bromine is removed with 10% sodium thiosulfate aq solution and reaction mixture is washed with water after the end of this reaction. The organic layer can be used for the methylamination reaction (yield ~140% MDP1P) or distill off DСM under vacuum to a solid.
The synthesis is conducted under normal conditions. 2-Bromo-3,4-methylenedioxypropiophenone 10 g from previous step is dissolved with n-methylpyrrolidone 50 ml in the reaction flask. The mixture is stirred until solids are dissolved.
Methylamine aqueous 40% 20 ml is added to the mixture, the flask is closed and stirred vigorously. Exothermic reaction have to be controlled. The reaction ends in 10 min and temperature decrease.
The exothermic reaction can be very violent and a forced cooling is necessary in case of large load. The flask should be immersed into a cold water bath for cooling. It is important to keep the temperature below 55 ºC.
The exothermic reaction can be very violent and a forced cooling is necessary in case of large load. The flask should be immersed into a cold water bath for cooling. It is important to keep the temperature below 55 ºC.
Methylone free base purification
The reaction mass is washed with sodium bicarbonate solution after reaction end, which is prepared in advance (water 120 ml and sodium bicarbonate 12 g). Sodium bicarbonate solution is poured into the reaction mixture and stirred vigorously for 1-2 min.
The reaction mass is washed with sodium bicarbonate solution after reaction end, which is prepared in advance (water 120 ml and sodium bicarbonate 12 g). Sodium bicarbonate solution is poured into the reaction mixture and stirred vigorously for 1-2 min.
Dichloromethane (CH2Cl2) 30 ml is added and stirred vigorously for 5 min. Methylone free base is extracted by DCM from this mixture. Organic layer is separated with help of separatory funnel.
Extraction
Layers separation in separating funnel (Photo 1). The bottom layer is DCM extract with cathinone base. The aqueous fraction is top layer, which have to be separated and extracted one more time with DCM 30 ml (Photos 2-3-4). The lower organic layers are combined and washed with distilled water 60 ml 3-4 times in separatory funnel until the methylamine smell absent (Photo 5-6). Methylone free base in DCM is always in the bottom layer. Layers are separated carefully. Try to avoid getting water into the organic layer. Organic solution is dried over MgSO4.
Layers separation in separating funnel (Photo 1). The bottom layer is DCM extract with cathinone base. The aqueous fraction is top layer, which have to be separated and extracted one more time with DCM 30 ml (Photos 2-3-4). The lower organic layers are combined and washed with distilled water 60 ml 3-4 times in separatory funnel until the methylamine smell absent (Photo 5-6). Methylone free base in DCM is always in the bottom layer. Layers are separated carefully. Try to avoid getting water into the organic layer. Organic solution is dried over MgSO4.
Acidification
Methylone free base solution in DCM is diluted with an equal volume of dry acetone (Laboratory grade 99%+). Then hydrochloric acid (~35%) is added in small portions dropwise. The mixture is stirred constantly and pH is controlled. A precipitate is appeared. If the mixture became very thick, acetone is added.
Methylone free base solution in DCM is diluted with an equal volume of dry acetone (Laboratory grade 99%+). Then hydrochloric acid (~35%) is added in small portions dropwise. The mixture is stirred constantly and pH is controlled. A precipitate is appeared. If the mixture became very thick, acetone is added.
The mixture must be very liquid in order to acidify methylone properly. When pH is reached 5.5-6, HCl addition is stopped. The mixture is cooled and filtered.
If methylone hydrochloride is not pure enough, you can read how to purify it here. Large crystals producing is described in this article.
Methylone hydrochloride purification with dry acetone gives a good result. There are several pictures of methylone hydrochloride before and after purification procedure.
Methylone hydrochloride purification with dry acetone gives a good result. There are several pictures of methylone hydrochloride before and after purification procedure.
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You use a lot of DCM here, I don't like it, can I replace it with anything else? (Ether?)
