After some failures due to my lack of patients finally got some good results thanks to
@William Dampier @Marvin "Popcorn" Sutton and passive spectator
@G.Patton
My first batches were pretty shit because I rushed too much and didn't use appropriate equipment. For instance I used 250ml drip funnel and I waited only for couple of minutes for the layers separation because I wanted to finish asap and that was the result (1st picture) , I'm gonna blend it, rinse it and crystallize it.
For the first batches I used BK4 and MA40%
After few fuck ups things started getting better, recipe changed a little bit because there are some issues with MA40% but I feet comfortable with current method.
Current method is cold synthesis, works good for me:
500g BK4 is dissolved in 1500ml DCM in 6L flat bottom flask using magnetic stirrer
500g of NaOH is dissolved in 1L H2O cooled (about 10 C) down and added to the flask
750g MA HCl is added to the flask in small batches so the temperature doesn't raise too much, roughly 100g - 150g every 10-15 minutes
The lid is closed and it's left for 16 - 24h hours on the stirrer
After that salt has to be filtered with buchner funnel, then the layers separated prepared for washing.
For first washing I use 3L filtered water with 150g sodium bicarbonate heated up to 30 C
Second washing just 3L of filtered water.
Once it's washed I use about 160ml and 800ml acetone for acidification and to get mephedrone powder, once pH 5 or lower is reached I put it to the freezer and leave overnight.
On the next day I filter as much as possible and leave it to dry. When I skipped that and filtered still wet mephedrone the yield was 240g, yesterday I done it Marvins way and it was 258g.
Marvins way
1. Filter
2. Dry
3. Rinse (cold acetone)
4. Dry
5. crystallize
Crystallization
1:2 powder mephedrone to water and alcohol 50% of the amount of water
I just pour the water to the pyrex glass bowl add mephedrone heat it up until little bubbles appear, boil for 5 minutes, switch the heating off and add alcohol the pour it to the crystallization dish and wait.
So if we compare how it stared and how it's going it's a big difference.