Alpha-PVP synthesis (1-10kg scale). Complete video tutorial.

[Ukspice]

@William Dampier

Need help with measurements

Instead of using :Valerophenone
I will buy liquid : 2-Bromovalerophenone

If I want to use 1litre

2-Bromovalerophenone​

What is the reagents amount I will need per I litrre:


-Hydrobromic acid (HBr) 48%;?

-Hydrogen peroxide (H2O2) 35%;?

-Pyrrolidine (CAS 123-75-1);???

-Ethyl acetate ;???

-Sodium carbonate (Na2CO3) 20% aq solution;???

-Diethyl ether (Et2O) ????

-EtOH 50 ???

-Dibenzoyl-D-tartaric acid ??

-Dichloromethane (CH2Cl2) 830 mL;

-Hexane ????

Hydrochloric acid conc. 35% (HCl);.??

WOULD REALLY HELP IF YOU CAN GET ME MEASUREMENTS FOR USE OF 1 LITRE 2-BROM. PLEASE?????

So that I can cost per reaction, also is the yield estimate about 20% loss
1 litre = 800g a-pvp?

 

[Marvin "Popcorn" Sutton]

I wrote you a PM.

 

[Taiwan]

Hi, I have the same problem, can you help?

 

[viking1111]

Hello i have little problem, for 25k 2bromovalero i use to crysyalization after pirolidyne and after washing, i use to crystalization 1,5l aceton to 0,38 acid per 1kg bromo, but liquid to crystalization i take 1l and make ph 2 with mixture of aceton and acid, after 10h in freezer nothing happend (it was mixing 4 hours with pirolidyne on temp 55) what i did wrong and how to fix it?

 

[Marvin "Popcorn" Sutton]

I suggest we go to private messages and discuss the details with synthesis.

 

[Taiwan]

Hi, I have the same problem, can you help?

 

[TERMOBAR]

Good evening, excuse me, can I ask you for help? I made a synthesis of Alfa pvp based on this recipe https://bbforum.eu/tags/a-pyrrolidinovalerophenone I did everything as described, except for distilling ethyl acetate, I brought the acidification to 5, put it in the freezer, and the salts did not fall out, how can I fix the situation?Next, I evaporated the solution to 1/2 at a temperature of 74-77 and put it in the freezer again and all without result, maybe someone has encountered this?Please help me!

 

[WillD]

If there is acid, you need to evaporate at low temperature or under vacuum. You can get the remains like black resin. You must use chemically pure dry acetone to crystallize this. If it is household acetone, then there may be problems. In addition to acetone, there is also a purifying method if you can get the resin and dissolve it in water. Extract the water with a solvent from impurities and crystallize the product from an aqueous solution when cooling.

 

[CalvinCandy]

Did you do it like the video?

 

[TERMOBAR]

Good day, thank you for your help, everything worked out for me, the whole problem, as I understand it, was in ethyl acetate after its complete spoilage and dilution with dry acetone, I was re-acidified and then the salts fell out.