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...

 

[G.Patton]

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...

darkmatter7You can make it without rotovap but it will take much more time.

 

[EvilC415]

Hoping I can get some help... I have had successfully rub multiple times but my last 2 are acting odd. Not sure what the issue is as all reactions have happened but no crystals have formed. Currently in freezer and 2 layers separated. Please reply and I can give more ino... thank you in advance...

 

[TheNut22]

Can hydrochloric acid be used to make 2-chloro valerophenone in same way as hydrobromide?
If not, can hydrochloric acid be used with copper(II)chloride to do the alpha chlorination?

 

[G.Patton]

Can hydrochloric acid be used to make 2-chloro valerophenone in same way as hydrobromide?
If not, can hydrochloric acid be used with copper(II)chloride to do the alpha chlorination?

TheNut22

Can hydrochloric acid be used to make 2-chloro valerophenone in same way as hydrobromide?Can hydrochloric acid be used to make 2-chloro valerophenone in same way as hydrobromide?Can hydrochloric acid be used to make 2-chloro valerophenone in same way as hydrobromide?

I don't think that it'll work. At least, you'll get much less yield.

 

[TheNut22]

I don't think that it'll work. At least, you'll get much less yield.

G.PattonMaybe this is better question, considering the same reaction:
If I use Copper(II)chloride, maybe with LiCl2 if I remember correctly, can that/those both reagent(s) be used to make that 2-chlorination, because alpha chlorination is made like that in many good reactions I've performed.

 

[G.Patton]

Maybe this is better question, considering the same reaction:
If I use Copper(II)chloride, maybe with LiCl2 if I remember correctly, can that/those both reagent(s) be used to make that 2-chlorination, because alpha chlorination is made like that in many good reactions I've performed.

TheNut22I can't answer you for sure. Carry out synthesis and figure out. Let us know your result.

 

[Lev]

Dear forum members. I need help. Where can I look at the synthesis of Valerophenone ?

 

[G.Patton]

Dear forum members. I need help. Where can I look at the synthesis of Valerophenone ?

LevHi, nowhere.

 

[WillD]

Benzene+AlCl3+Valeryl chloride