Síntese de alfa-PVP (escala de 1-10 kg). Tutorial completo em vídeo.

[GeneralX]

Hello.
I use for 10 grams of the final product:
2'-Bromovalerophenone (BvP): 10 г
Pyrrolidine: 4.2 ml
Ethyl acetate (EA): 20 mL
37% hydrochloric acid (HCl): ~0.69 mL
Distilled water: 20 ml
Acetone: 30 ml
At the stage when BvF+Ethyl acetate+Pyrrolidine I have the liquid separates into two layers, as on the photo

Spoiler: photo

 

[G.Patton]

Hello, you had to take more Pyrrolidine 7.67 ml.
Have you stirred the mixture for 1h? What about a temperature of the reaction?

 

[GeneralX]

I kept the temperature around 59-60 degrees. But not for a long time, about 10-15 minutes of stirring

 

[G.Patton]

You don't need to heat it, just avoid overheating during exotermic reaction of BVF with pyrrolidine.

 

[GeneralX]

But despite this, I further continued to acidify with 37% hydrochloric acid, having previously added 30 ml of cold acetone. But still nothing formed, so far I put it in the freezer, but I feel that nothing will form. ph always shows around 5. Please help me

Spoiler: photo

 

[G.Patton]

You had to evaporate EA after the reaction. It interferes to form a-PVP HCl crystals.

 

[GeneralX]

What are some easy ways to vaporize Ethyl Acetate?

 

[dnBQByvHb8Zkawbjpx]

Boil it off in vacuum.

 

[Polka999]

Is your acetone distilled?

 

[GeneralX]

All right, thank you. I'll try again.