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]

Add acetone and put in the freezer for a day

 

[w2x3f5]

The 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

 

[savage36]

Mines to

 

[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]

You 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]

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

 

[TheNut22]

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.

 

[G.Patton]

I 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]

Hi, nowhere.

 

[WillD]

Benzene+AlCl3+Valeryl chloride

 

[scared]

hello
i read that pyrrolidine can be substituted b Metilamine.
some one can tell me if is it correct and witch proportios it is substituted.
1000 ml of pyrrolidine can be reemplaced by 1000 ml Methilamine hcl or how much 40% water solution

thanks for advanced

 

[xirmsx12]

Yo I tried with hexanophenone and it didn't seem to work the same as when I used valerophenone. Is it a heating issue, mixing issue, or what? I couldn't get the pyrrolidine to react properly to get a decent freebase of APHP in case anyone is reading this. It ended up being almost inactive. Equipment used was almost all there shy of the reflux condenser.

 

[WillD]

PHP is usually more difficult to crystallize. But in general, there should be no problems. You can clarify this with me, but not in this topic.

 

[Skurczolo]

After mixing bromoket in ethyl acetate with pyrrolidine i have to destille ethyle acetate from top layer under vacuum ?

 

[WillD]

If you can evaporate ethyl acetate with vacuum and mix the base with dry acetone, this is a very good method

 

[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.