My 3-CMC synthesis

[draconic123]

After washing dirty 3cmc powder with acetone and recrystallizing with 1:2 water acetone mixture all i've got is white goo like substance and no crystals forming, any ideas?

 

[Jesse_Pinkman_]

After washing dirty 3cmc powder with acetone and recrystallizing with 1:2 water acetone mixture all i've got is white goo like substance and no crystals forming, any ideas?

draconic123That happens when you have moved the container and the solution came in motion, Just let it stand there for a few days and wait.

 

[draconic123]

ive got a question about ethyl acetate, when i did the reaction with DCM, the crystals turned out to be quite clean and the resulting weight was quite good aswell, however with ethyl acetate, it seemed like there still was unreacted 2b3c, im unsure whether i have to put in more solvent or methylamine, but the crystals came out really dirty and oily using ethyl acetate. do u guys have any opinions?

 

[Bazooka90]

ive got a question about ethyl acetate, when i did the reaction with DCM, the crystals turned out to be quite clean and the resulting weight was quite good aswell, however with ethyl acetate, it seemed like there still was unreacted 2b3c, im unsure whether i have to put in more solvent or methylamine, but the crystals came out really dirty and oily using ethyl acetate. do u guys have any opinions?

draconic123The boiling point of ethyl acetate is 77°celsius.what temperature did u set?

 

[Bazooka90]

ive got a question about ethyl acetate, when i did the reaction with DCM, the crystals turned out to be quite clean and the resulting weight was quite good aswell, however with ethyl acetate, it seemed like there still was unreacted 2b3c, im unsure whether i have to put in more solvent or methylamine, but the crystals came out really dirty and oily using ethyl acetate. do u guys have any opinions?

draconic123The boiling point of ethyl acetate is 77°celsius.what temperature did u set?

 

[Athanasias]

@Jesse_Pinkman_ thank you so much for contributing all of the information. It was of great benefit to me on my first attempt with 4mmc. I used 2b4m(50g), EthylAcetate and methylamineHCL. It was a small run as I didn’t want to waste. I yielded around 45%.
Overall, I’m very pleased and look forward to fine tuning everything. Thanks again!