Question - recrystalization

[noMercyy]

Can some one explain why 3cmc after recrystalization occurs white over short time and how can i get permament glass look crystals? i tried in ipa, aceton and only water. The results of it are very satisfying but that occurs white over time is the main problem. Next problem is brownish spots on the top of crystals. Any one have solutions/advices for me? I read all of 4mmc crystalization topic, and dont find any help.

 

[azides]

First. Did you use filter paper and filtering to get all the hair and junk first?

Second. How quick are you doing recrystalizations? I notice when usually working with amines or even 4mmc. After multiple recrystalizations on the final one they can be white. But to go from sugar to glass. I go slow. Like weeks/months ..

Ps I had also done multiple recrystalizations from dh20 as well was almost see thru mdma.the solute was clear concentrated..Recrystalizations after in acetone or ethanol brown reappeared... take that for what you will with amines

 

[HectorFromTroy]

First. Did you use filter paper and filtering to get all the hair and junk first?

Second. How quick are you doing recrystalizations? I notice when usually working with amines or even 4mmc. After multiple recrystalizations on the final one they can be white. But to go from sugar to glass. I go slow. Like weeks/months ..

Ps I had also done multiple recrystalizations from dh20 as well was almost see thru mdma.the solute was clear concentrated..Recrystalizations after in acetone or ethanol brown reappeared... take that for what you will with amines

azidesI would like to add something to this. From my experiments I noticed that 4mmc tends to be hesitant to precipitate and crysalize this can be because of excess methylamine or other products from side reactions but either way for some reason I found out that leaving it in a colder place like the fridge encourages crystallization

 

[azides]

But when I go slow it makes clear big rocks

 

[WillD]

The remains of the crystallization solution dry on crystals and therefore crystallize the remains of the product in the form of a small surface powder. You need to thoroughly rinse with dry acetone crystals to remove the crystallization solution completely. Acetone should be very cold to avoid dissolving the surface of the crystals. Drying of the crystal will be better under the conditions of a vacuum (using a desiccator as an example)