Hi..
I just converted 2-bromo-3-chloropropiophenone with DCM and Methylamine 40% aq. Reaction succeeded. Now the crystalization part. It seems to be more tricky than other cathinones.
You described. To add 50ml of water to your EthylAcetate/3-cmc freebase. Then add 30ml of 35% hcl to 50ml of water. Add it dropwise until pH = 5.0-6.0
Question 1: did you at any point observed any separation line? The natural thing to happen would be that the EthylAcetate layer would be separated into the upper layer.
Question 2: what temperature did your mixture reach after 12 hours of sitting in the freezer? It should not go below 0° celcius as there is a substantional amount of water present.
So if I am correct then my DCM+freebase just needs water. Then adjust pH to 5.0-6.0, freezer for 12 hours and that's it
I just converted 2-bromo-3-chloropropiophenone with DCM and Methylamine 40% aq. Reaction succeeded. Now the crystalization part. It seems to be more tricky than other cathinones.
You described. To add 50ml of water to your EthylAcetate/3-cmc freebase. Then add 30ml of 35% hcl to 50ml of water. Add it dropwise until pH = 5.0-6.0
Question 1: did you at any point observed any separation line? The natural thing to happen would be that the EthylAcetate layer would be separated into the upper layer.
Question 2: what temperature did your mixture reach after 12 hours of sitting in the freezer? It should not go below 0° celcius as there is a substantional amount of water present.
So if I am correct then my DCM+freebase just needs water. Then adjust pH to 5.0-6.0, freezer for 12 hours and that's it
- By G.Patton
Hi, freezer temp is usually about -15*C. It's okay. Water is in the mixture.
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Will the DCM and water layer not seperate? Then ice will be formed in water layer in the freezer. Is it not easier to acidify, then separate water layer. Slowly evaporate water layer?..
- By G.Patton
If ice will be formed during crystallization, it won't spoil the reaction product. Please, follow the method:
10. Next, the mixture is poured into a 2 L beaker and the beaker is put into a freezer for 12 h.
11. A vacuum filtration system (Buchner flask and funnel, vacuum pump) is assembled.
12. The vacuum pump is turned on.
13. The crystalline beaker content from freezer is poured onto the Buchner filter.
14. The cold 3-CMC solution is filtered and pressed until the funnel content is become solid.
10. Next, the mixture is poured into a 2 L beaker and the beaker is put into a freezer for 12 h.
11. A vacuum filtration system (Buchner flask and funnel, vacuum pump) is assembled.
12. The vacuum pump is turned on.
13. The crystalline beaker content from freezer is poured onto the Buchner filter.
14. The cold 3-CMC solution is filtered and pressed until the funnel content is become solid.