Síntese de alfa-PVP (escala de 1-10kg). 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

 

[Polka999]

Is your acetone distilled?

 

[GeneralX]

My acetone is cold and 99% acetone. What do you mean, discylated?

 

[Polka999]

Yes i asked if your acetone was pure.
One more question.
Pictures that you uploaded, at what stage is that picture taken
After removing it from freezer or after adding pyrro & distilled water?

 

[GeneralX]

In the first picture is when after adding bromvaleraphenone+ethyl acetate+pyrrolidine, and remixed for 20-30 minutes at 59 degrees.

 

[Polka999]

I re-watched video. That dark oil should be on top not bottom. You are doing something wrong at that stage.

 

[Polka999]

Also did you heated it? since it does not need any heat (it will self heat after adding pyrro)

 

[GeneralX]

Here are my proportions I use for 10 grams of alpha pvp:
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

 

[GeneralX]

Yeah, on the magnetic stirrer, I raised the temperature a little bit to get to 60 degrees.

 

[Polka999]

Well raising temperature is not needed. Pyrrolidine will rise temperature by itself.
After adding pyrro, add distilled water and that dark oil should form on top not bottom.

 

[GeneralX]

Immediately after adding the pyrrolidine, do you have to add the discylated water?

 

[Polka999]

After adding all pyrro (You should add pyrro drop by drop very slowly so it won't overheat) you should mix it for 25-30 min. Color will change from yellow to orange. After 25-30 min of mixing you should add distilled water immediately and continue mixing for 5-10 more min.

After that liquids will get separated. On top should be orange liquid. On bottom yellow liquid. You should collect orange liquid on top.

 

[GeneralX]

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

 

[lapgan1]

heat it to evaporate all the ethyl acetate, you will see a layer of oil, add cold acetone and add hcl you will get a precipitate, but I got quite little precipitate and the powder melted when left for a while

 

[GeneralX]

I after adding bromvaleraphenone+ethyl acetate+pyrrolidine at 59 degrees for about 10-15 min stirring. At what temperature should I stir and for how long?

 

[lapgan1]

I just put it all in a bottle and shook it for an hour after adding the pyrrolidine

 

[GeneralX]

And did you have a homogeneous mass afterward?

 

[lapgan1]

if you use less ethyl acetate, it will separate into two layers when pyrrolidine is added i think

 

[lapgan1]

The lower layer maybe is pyrrolidine because it is water soluble

 

[GeneralX]

But in the video, after adding pyrrolidine, the liquid does not separate into two layers. But in my video, after adding pyrrolidine, the liquid separates into two layers. Although the liquid should separate into two after adding discylated water

 

[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.