hello people, so i've been doing 3cmc synth with ethyl acetate and i'm acidifying freebase with water, 3cmc doesnt precipitate when acidifying freebase only for some reason... regardless, i was wondering whether it would be possible to add IPA before acidification in order to get clean crystals in one go, or would it ruin the reaction?
question about 3cmc synth
- Thread starter draconic123
- Start date
I had also results with acidification in freebase only but were not as good as with water together and evaporate the water layer.
Recrystallisation after acidification should be possible but if the crystals are cleaner then, i can not say.
Recrystallisation after acidification should be possible but if the crystals are cleaner then, i can not say.
- By draconic123
Have you ever tried reaction with 2 solvents? Im gonna buy some nmp and try with nmp and ethyl acetate.. should be much more clean and more crystals
op
What temperature did u use for ethyl acetate reaction?
What temperature did u use for ethyl acetate reaction?
No temp control needed, just mix and stir for 20min... temp rises and falls from the reaction itself
Upload the synthesis your following
- By draconic123
Im doing what jesse pinkman is doing in his post except im adding 5:1 ratio of ethyl acetate to 2b3c, im thinking of acidifying rm with less water and some ipa because right now I add same amount as rm and clearly its too much and slows down crystalization