3cmc freebase acidification

[draconic123]

I've been doing 3cmc synthesis with both organic and water layer successfully for quite some time now, however I keep having trouble with freebase only. I tried ethyl acetate and dcm with same results. After draining water layer, I add acetone and start acidifying slowly. Rm quickly darkens and black blobs of water from acid appear. I reached ph of 6, stored the freebase in room temperature for a bit of evaporation and the color became yellow again with no precipitation whatsoever. Haven't had any problems with both freebase and water together.. any ideas?

 

[Jesse_Pinkman_]

I've been doing 3cmc synthesis with both organic and water layer successfully for quite some time now, however I keep having trouble with freebase only. I tried ethyl acetate and dcm with same results. After draining water layer, I add acetone and start acidifying slowly. Rm quickly darkens and black blobs of water from acid appear. I reached ph of 6, stored the freebase in room temperature for a bit of evaporation and the color became yellow again with no precipitation whatsoever. Haven't had any problems with both freebase and water together.. any ideas?

draconic123Why do you want to do this?
I see no sense in it, you cant evaporate freebase and expect that crystals will form...you can put it into freezer but the results are not the same as with water

 

[draconic123]

Why do you want to do this?
I see no sense in it, you cant evaporate freebase and expect that crystals will form...you can put it into freezer but the results are not the same as with water

Jesse_Pinkman_I dont want to get crystals, I want to get powder faster. So I could clean it because crystals all come out dirty anyway.

 

[Jesse_Pinkman_]

I dont want to get crystals, I want to get powder faster. So I could clean it because crystals all come out dirty anyway.

draconic123Crush the crystals to powder with mixer, wash then, recrystallisation

 

[w2x3f5]

I've been doing 3cmc synthesis with both organic and water layer successfully for quite some time now, however I keep having trouble with freebase only. I tried ethyl acetate and dcm with same results. After draining water layer, I add acetone and start acidifying slowly. Rm quickly darkens and black blobs of water from acid appear. I reached ph of 6, stored the freebase in room temperature for a bit of evaporation and the color became yellow again with no precipitation whatsoever. Haven't had any problems with both freebase and water together.. any ideas?

draconic123you have problems at the ketone bromination stage,