3-CMC Synthesis Question

[Jesse_Pinkman_]

This is what i got

 

[antrax]

Hi! my friend, How do you get transparent crystals after recrystallization?
I have synthesized methylone but after recrystallization I obtain orange-brown crystals and that I think means that the methylone crystals have impurities.
Thank you!!

 

[Jesse_Pinkman_]

I dont use acetone at all, only for washing...you have 2 options, acidificaction(only icecold hci 37%) with freebase+water or only freebase.
I recomend with water. Then evaporate the water or freebase.
Thats it.

 

[Jesse_Pinkman_]

I dont use freezer method, but i tried and had different results.

 

[letsrunfast]

Does the freebase+water make an emulsion with stirring? If it does, is it easy to break the emulsion? I wonder why acetone does not work for acidification for 3-cmc. Lol. It makes the 3cmc very dark.

 

[Jesse_Pinkman_]

I did it several times, but you need to take much time for acidificaction, especially without acetone, i use a drip funnel, every 2-3 seconds 1 drop. Takes 30min sometimes. And the solution has to be stirred all the time, magnetic stirrer works good till aprox 1 Liter.
I never got an emulsion, just 2 layers.

 

[Jesse_Pinkman_]

Try without acetone, but how i said, choose your layer, if freebase, then dont use additional water, but i prefer with water. But both is possible

 

[letsrunfast]

Did you dilute the HCL with additional water? Or kept the original concentration of ~37 percent strength?

 

[Jesse_Pinkman_]

I used it directly from the bottle, but kept it in the freezer before. You should use cold dest.water too, which will be added to the freebase, to keep a low temp while acidificaction