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Purification of mephedrone powder.

Marvin "Popcorn" Sutton

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The synthesis of mephedrone produces reaction byproducts and leaves unreacted precursor residues. It is necessary to purify a product with insufficient purity to reduce health risks.

Once the free base of the mephedrone is oxidized, the mixture must be converted to a liquid state. Too thick a mixture is slow to filter, the product clogs the filter, resulting in a paste that looks like clay. Such a mass contains many impurities. It has a pungent chemical odor. Color that is different from normal. It may not harden for a long time. Therefore, it is important to remove as much liquid as possible, preferably to a crumbly state, by gently stirring the product on the filter with a spatula. If necessary, if the product is visually contaminated, a little ice-cold acetone can be added to the filter (the colder, the better). After straining, it is very important to dry the product thoroughly so that it is crumbly and does not stick to lumps. You can use an infrared lamp (infrared heater) or a drying cabinet for drying. After drying, be sure to sift the product to make sure it is dry enough. You will have a powdery fraction.

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The quality of the powder is checked with a solution in water: 1 g is dissolved in 3 ml of 100 ºC water (you can use water from a kettle). The procedure is carried out in a transparent container so that you can see the quality of the solution. The solution should be clear and colorless. If insoluble particles or a dark color (darker than lemon) are present, additional purification of the product is necessary. The darker the color, the more impurities the mephedrone contains.
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Cleaning with acetone:
Place the mephedrone evenly over the filter area and pour ice-cold acetone on top, so that the acetone layer covers the product by 2-3 cm and turn on the vacuum. Filter to a crumbly state, distilling off the liquid as much as possible, in the process, you can gently stir with a spatula. Add acetone, in small portions, until clear liquid in the flask receiver. Then dry well, sift, and repeat dissolving in water.
*A very high quality 99%+ acetone is best for purifying mephedrone powder. Sometimes a small amount of dichloromethane or ethyl acetate is washed before acetone.

Recrystallization in isopropanol:
Place a glass or enameled container on an electric stove (use an electric stove only, isopropanol is very flammable). Pour isopropanol and turn on a gentle heat to 80 ºC. When the temperature reaches a slight boil (small bubbles), start adding mephedrone in small portions with stirring, so that everything dissolves. Do not let the mixture boil too much, turn off the heat if necessary, so as not to spoil the product. Once the product stops dissolving, we will have a saturated solution of mephedrone in isopropanol. We take the solution off the heat and cool it to room temperature, then 8 hours in the refrigerator and 8 hours in the freezer. As a result, we get a clear precipitate, all the dirt remains in the isopropanol. The precipitate is filtered under vacuum. Compare the mass of the obtained mephedrone with the deposit before recrystallization. If the losses are big (>50%), probably part of the product is still in isopropanol. In this case we evaporate the isopropanol by 50% and slowly cool and filter again.

Purification of mephedrone solution in dichloromethane.
Dissolve mephedrone in the proportion of 1 g per 1 ml of water (+30 ºC), add 0.5 volume of dichloromethane and stir the solution well for a few minutes. Allow to stand and observe the separation into two fractions: the upper aqueous layer - the mephedrone solution, the bottom layer - dichloromethane with impurities. We separate the upper layer, dispose of the lower one. The mephedrone aqueous solution can be evaporated to powder, or it can be used to grow crystals. Washing the mephedrone solution can be done several times until the solution becomes colorless.

The methods provided can be used in combination. After you have obtained a high-quality powder, I recommend that you crystallize - http://bbzzzsvqcrqtki6umym6itiixfhn...threads/crystallization-of-mefedrone-4mmc.72/
 
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