Mostly I use 99.9% purity acetone from a chem shop.
All normal product gone, and raw material for new batch has not arrived, so I had some free time and nothing to do.
So, I gathered dirty acetone I had in the freezer, in the amount 2L and evaporated it. Mostly it was acetone that was used for MDMA crystals washing, but some volume (relatively small amount may be 15-20%) was after acidation with 37% HCl in acetone that I really love.
Evaporation was done on the hotplate in the beaker of 1L, then some extra amount was added in a few steps. Final evaporation was done in the beaker 100ml. I din't control the temperature in the beaker, just set the temperature of plate surface as 150C. All the process didn't take a lot of time, may be 1 hour or something of intensive boiling.
At the point when acetone smell disappeared, I had small volume of shitty black dense liquid, that was mixed with small volume of water and put in the freezer for an hour or something.
Then NaOH was added for base extraction. Upper layer, pretty dirty and black, was separated on funnel its weight was exactly 25 gr, that's not bad for 2L of acetone.
Then NaCl and distilled water were added to the funnel with upper layer and kept in the freezer for some more time. Product washed with p.ether. That after evaporation gave me 15 gr of pretty pure FB.
FB was acidified in frozen acetone and filtered after 12 hours. Yeld was 16.8 gr against calculated 17.8 gr.
The salt was re-crystallized in hot IPA in the sealed PP beaker on water bath - it is very easy to control the temperature of water bath. Starting temperature was 65C, proportions by weight 1 gr : 2.86 gr (or 3.6 ml at RT). As I don't have programmable hotplate, I had to do it manually, reducing temperature for 2C every 30 minutes.
As RT was reached, sealed beaker together with water pan (to reduce speed of cooling) were placed in the normal refrigerator for 6 hours, then moved to the freezer for a few hours more.
As the result, 15.2 gr of pretty pure crystals were obtained. But average cr size doesn't impress me. It is still small 1x1 up to 2x3 mm. Probably re-crystallization with steps 2C per 30 minutes is still too fast, I think I need to buy a programmable plate and do the same with 1 or 2C per 1 hour.
All normal product gone, and raw material for new batch has not arrived, so I had some free time and nothing to do.
So, I gathered dirty acetone I had in the freezer, in the amount 2L and evaporated it. Mostly it was acetone that was used for MDMA crystals washing, but some volume (relatively small amount may be 15-20%) was after acidation with 37% HCl in acetone that I really love.
Evaporation was done on the hotplate in the beaker of 1L, then some extra amount was added in a few steps. Final evaporation was done in the beaker 100ml. I din't control the temperature in the beaker, just set the temperature of plate surface as 150C. All the process didn't take a lot of time, may be 1 hour or something of intensive boiling.
At the point when acetone smell disappeared, I had small volume of shitty black dense liquid, that was mixed with small volume of water and put in the freezer for an hour or something.
Then NaOH was added for base extraction. Upper layer, pretty dirty and black, was separated on funnel its weight was exactly 25 gr, that's not bad for 2L of acetone.
Then NaCl and distilled water were added to the funnel with upper layer and kept in the freezer for some more time. Product washed with p.ether. That after evaporation gave me 15 gr of pretty pure FB.
FB was acidified in frozen acetone and filtered after 12 hours. Yeld was 16.8 gr against calculated 17.8 gr.
The salt was re-crystallized in hot IPA in the sealed PP beaker on water bath - it is very easy to control the temperature of water bath. Starting temperature was 65C, proportions by weight 1 gr : 2.86 gr (or 3.6 ml at RT). As I don't have programmable hotplate, I had to do it manually, reducing temperature for 2C every 30 minutes.
As RT was reached, sealed beaker together with water pan (to reduce speed of cooling) were placed in the normal refrigerator for 6 hours, then moved to the freezer for a few hours more.
As the result, 15.2 gr of pretty pure crystals were obtained. But average cr size doesn't impress me. It is still small 1x1 up to 2x3 mm. Probably re-crystallization with steps 2C per 30 minutes is still too fast, I think I need to buy a programmable plate and do the same with 1 or 2C per 1 hour.
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