Sintesi dell'alfa-PVP (scala 1-10 kg). Video tutorial completo.

[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.

 

[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...

 

[GeneralX]

Spoiler: bromvaleraphenon

Hello, I ordered bromvaleraphenone CAS: 49851-31-2 from China and this is what I got. Does it look like bromvaleraphenone at all? It's brown in color.

 

[William D.]

It doesn't look the best. Try to mix part with a aqueous solution of soda and see how it will react.

 

[Polka999]

How it should react?

 

[lamename69]

He, can I ask about the reflux condenser used in the video? I'm no lab rat so the question that comes to my mind is what is the purpose of having a reflux condenser in one of the holes if there is a wide-open hole for the fumes to go out where the stirrer is?

Another question, can we racemize the foul isomer of a-PVP in order to keep retrieving it?

 

[William D.]

u can do without a condenser, the synthesis can be done in a regular bucket. There is no point in separating isomers.

 

[KANISTRO_RUTOR]

Good afternoon, how can I check the quality of 2-bromvalerophenone?
2-bromocalerophenone was purchased and the reaction does not start, the weight and boiling point do not match. How can the seller prove that it is not 2-bromocalerophenone How to find out what it is 2-bromvalerophenone

 

[Polka999]

Good question. Please let us know how to check quality of 2-bromo if it's even possible.
@William D. @Marvin "Popcorn" Sutton @G.Patton

 

[G.Patton]

Hello. Sorry for a long reply.
GC-MS analysis can determine what is it. What is a difference in bp of your liquid and literature data?

 

[KANISTRO_RUTOR]

@William D.

 

[William D.]

DM

 

[SpaceRocket]

hello, I have a question, I have all the steps. followed the process and have a nice a-pvp with a result of 80%. I do it on a larger scale between 1 and 0.5 kg bromo, but now I wonder how I can get large, beautiful crystals because if I try to recrystallize in water it grows. back like little needles. You can see on the picturen powder what i have made and the cristals sombody els but he dont want to tel me how he did it if sombody can help me wild be great!!!

 

[G.Patton]

Salve, come si ricristallizza?

 

[SpaceRocket]

I am loking for method how to cristalize , when i want to cristalize i get nedel cristal like this on the photo

 

[G.Patton]

a-PVP crystallization

 

[brazil_guy]

The good thing about pvp is that all raw materials to Synthesize is legal to buy in my country

 

[RegulierTier]

Can I replace the ethylacetate with toluene or TBME?
I don't have a rotovap so destill under vacuum would be a problem...

 

[SpaceRocket]

I did it with 2 infrared lamps and had to evaporate 16.9 ethiel acetate in plastic containers, which took me 30 hours and i dry my powder also with the lamps that go very fast in view hours your powder is dry