3-CMC Synthesis Question

[Jesse_Pinkman_]

This is what i got

 

[antrax]

This is what i got

Jesse_Pinkman_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_]

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.

letsrunfastI 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_]

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.

letsrunfastTry 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]

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

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

 

[Jesse_Pinkman_]

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

letsrunfastI 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