Alfa-PVP süntees (skaala 1-10kg). Täielik videoõpetus.

[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.

 

[G.Patton]

Hi, for a what reason do you assume to add water there? Yes, you can heat the solution to 100*C but take into account that it's not okay for free base. It also will be evaporated partly. It's worth to use vacuum distillation!

 

[Bitwise]

vacuum distillation seem to bit a little .... expensive to me.
sadly i just cant afford them...