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

[getmoneyforlife]

Hi. I have a problem with crystallization. After adding hydrochloric acid, the reaction does not crystallize. When you first start mixing the 2bromovalerophenone with the ethyl acetate and prolidine, it looks like it didn't mix well. The mixture was stirred for 1 hour. The layers have separated and it shouldn't be like that. Only later did I add distilled water and the phases separated, but why does it look so bad at the beginning?
Proportion:
*2bromovalerophenone ~760ml
* ethyl acetate 4L
*pirolidyna 1L
*water distillate 6L
*Aceton 4L
*ACID 36% 200-300ml

 

[w2x3f5]

Hi. I have a problem with crystallization. After adding hydrochloric acid, the reaction does not crystallize. When you first start mixing the 2bromovalerophenone with the ethyl acetate and prolidine, it looks like it didn't mix well. The mixture was stirred for 1 hour. The layers have separated and it shouldn't be like that. Only later did I add distilled water and the phases separated, but why does it look so bad at the beginning?
Proportion:
*2bromovalerophenone ~760ml
* ethyl acetate 4L
*pirolidyna 1L
*water distillate 6L
*Aceton 4L
*ACID 36% 200-300ml

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getmoneyforlifeAdd acetone and put in the freezer for a day

 

[w2x3f5]

Ok, . But the bigger problem for me is why are the layers separated at the beginning when mixing? I'm not talking about the stage when I add distilled water to separate the layers

getmoneyforlifeThe problem is that you wrote 4 liters of ethylacetate and etc in the description, but the photo is an order of magnitude less, and you also did not write your work by steps with your observations. I am not Nostradamus to warn your actions and the synthesis itself. Crystallization turned out as I see.

 

[getmoneyforlife]

I have 2 questions.
Why did this liquid start to separate or not mix?
Why did the solution not turn cloudy during acidification with hydrochloric acid?
I started doing it too quickly after a long break, I lost 1 kg, I made 2 samples of 50 g each, but something is not working out as it should. Efficiency 60% 40ml 2bromovalerophenone 50ml pyrrolidine

 

[islandgato]

How to evaporate? Mine it’s all liquid even 12 hours on freezer

 

[darkmatter7]

Do I really have to buy a rotovap?
Starting from nothing, what would be the initial cost of all this?

It's too bad it's so hard to simply find this stuff, that we have to make ourselves...