Introduction
Mephedrone (4-MMC) synthesis reaction is carried out with production of some amount by-products. Also, some amount of unredacted precursor is left in the reaction mixture after reaction. It takes to purify a 4-MMC product with insufficient purity to reduce health risks.
Manual
As soon as mephedrone hydrochloride is obtained, the mixture have to be turned into liquid state. It is hard to filter too thick mixture. The product can clogs Buchner funnel. A resulting product paste looks like clay, contains different impurities and has pungent chemical odor. A such product color is distinguished from usual. Also, it can solidify for a longer time. It is essential to remove as much as possible solvent from a product and it is better to reach a crumbly state, by gently stirring the 4-MMC product on the filter with a spatula. If the product is looks contaminated, a little dry ice cold acetone can be used for washing on the filter (the colder acetone, the better). It is important to dry the 4-MMC thoroughly so that it is crumbly and does not stick to lumps. Infrared lamp (infrared heater) can be used for drying in a dry warm room. The product have to be sifted to be sure that it is dry enough. You will obtain a powdery fraction.
Mephedrone (4-MMC) synthesis reaction is carried out with production of some amount by-products. Also, some amount of unredacted precursor is left in the reaction mixture after reaction. It takes to purify a 4-MMC product with insufficient purity to reduce health risks.
Manual
As soon as mephedrone hydrochloride is obtained, the mixture have to be turned into liquid state. It is hard to filter too thick mixture. The product can clogs Buchner funnel. A resulting product paste looks like clay, contains different impurities and has pungent chemical odor. A such product color is distinguished from usual. Also, it can solidify for a longer time. It is essential to remove as much as possible solvent from a product and it is better to reach a crumbly state, by gently stirring the 4-MMC product on the filter with a spatula. If the product is looks contaminated, a little dry ice cold acetone can be used for washing on the filter (the colder acetone, the better). It is important to dry the 4-MMC thoroughly so that it is crumbly and does not stick to lumps. Infrared lamp (infrared heater) can be used for drying in a dry warm room. The product have to be sifted to be sure that it is dry enough. You will obtain a powdery fraction.
The 4-MMC powder quality is checked with a solution in water: 4-MMC 1 g is dissolved in water 3 ml 100 ºC. This procedure is carried out in a transparent beaker so that you can see a solution color. The solution should be clear and colorless. If insoluble particles or a dark color (darker than lemon) is presented, additional purification of the product is needed. The darker solution color, the more impurities 4-MMC contains.
Acetone washing:
Mephedrone powder is placed into Buchner filter and dry ice cold acetone is poured. Acetone is poured during vacuum pump working. You have to avoid excess amount of acetone on the filter by reason that part of 4-MMC can be dissolved. Product have to be filtered to a crumbly state and acetone have to be removed as much as possible. You can gently stir 4-MMC with a spatula to reach the best result. Acetone is added in small portions until clear solvent in receiver flask is obtained. Then, the product is dried well, sifted, and checking procedure is repeated.
*Ahigh quality 99%+ acetone, which is distilled and dried before this procedure, is suitable for mephedrone powder purification. Sometimes a small amount of dichloromethane or ethyl acetate is washed before acetone.
Recrystallization in isopropanol
A glass or enameled container is placed on an electric stove (use an electric stove only, isopropanol (IPA) is easy flammable). IPA is poured and a gentle heating is turned on to 80 ºC. When a slight boiling (small bubbles) temperature is reached, mephedrone addiction is started in small portions with a stirring in order to dissolve all product. Do not let the mixture boil too much, the heater is turned off if it is necessary to avoid the product spoiling. As soon as product dissolving is stopped, a saturated mephedrone solution in IPA is obtained. The solution is cooled down to room temperature, 8 h in a fridge and 8 h in a freezer. As a result, a clear 4-MMC hydrochloride precipitate is obtained, a most by-products is remained in IPA. The precipitate is filtered with vacuum. Compare obtained 4-MMC mass with 4-MMC salt before recrystallization. If losses are too height (>50%), part of the product probably is still in IPA solution. In this case, ~50% IPA is evaporated, slowly cooled and filtered again.
Purification of the mephedrone solution in dichloromethane
Mephedrone is dissolved in ratio 1 g per 1 ml of water (+30 ºC), 0.5 volume of DCM is added and solution is stirred vigorously for few min. The solution is left for several min without stirring and two layers are formed. The upper aqueous layer is mephedrone solution, the bottom layer is DCM with by-products. Layers are separated, DCM layer is thrown out. The mephedrone aqueous solution can be evaporated to a pure powder or it can be used to crystals growing. The mephedrone solution washing can be done several times until the solution becomes colorless.
These methods can be used in combination. You will obtain a high-quality powder, It is recommended to make crystals http://bbzzzsvqcrqtki6umym6itiixfhn...threads/crystallization-of-mefedrone-4mmc.72/
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