Kissel place crystals a-pvp

[Zavarkin]

Hello, dear colleagues, I have a problem at the stage of crystals falling out after the oil has oxidized. We poured a-pvp into trays in ethyl alcohol and put it in the freezer, but instead of crystals we got something similar to jelly. How can this be fixed? Please help.

 

[G.Patton]

Hello, how have you synthesized and acidified a-PVP base?

 

[Zavarkin]

After adding Pyrrolidine to 20 liters of valerophenone, we washed the oil twice with water, separated the layers, poured in 15 liters of ethyl alcohol and acidified with hydrochloric acid to pH 5.5.

 

[G.Patton]

You had to use 2-bromovalerophenone for this synthesis.

 

[Zavarkin]

I apologize for writing incorrectly, 21 liters of pyrrolidine were added to 20 liters of 2-bromovalerophenone, after adding, 10 liters of methyl acetate were poured in, stirred for 4 hours, then the oil was washed with water twice, then it was poured into ethyl alcohol in the amount of 15 liters and we proceeded to acidification, when the pH mark became 5.5, we stirred the RS for another hour, then poured the RS into trays and put it in the freezer for 3 days, but instead of crystals, we got snot. Please tell me what we did wrong?

 

[Osmosis Vanderwaal]

I don't know anything but when I've read of similar situations it was the hydrophilic nature of ethanol and solubility of acid salts in water. Was it technical grade 99% ethanol? was it brand new? I'm just thinking out loud

 

[Neeto84]

try evap the alcohol and use acetone