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

[keras]

Can I acidify in water solutiom not with acetone? And evaporate water afterwards like with 4mmc?

 

[G.Patton]

You can use less concentrated HCl aq solution.

 

[G.Patton]

You can read a-PVP crystallization topic.

 

[RegulierTier]

Can I use toluene instead of Ethyl acetate so I don't need to use a rotary?

 

[G.Patton]

Hello, you can don't use it with EA as well.

 

[G.Patton]

You are not obligated to use rotovap in any case. Try to carry out synthesis in a small scale at first.

 

[RegulierTier]

Hey, i've made everything like in the Video but after I added Aceton and hcl to the freebase, it seperated into two layers. I've just put it to the freezer without seperating the two layers from each other. Is that okay?

 

[lapgan1]

I always have the same situation as you if I don't evaporate ethyl acetate, only when I evaporate ethyl acetate does it precipitate.

 

[RegulierTier]

Ok what should I do now? Just heat a bit and wait until some evaporated?

 

[lapgan1]

Heat until the odor of ethyl acetate is gone. use acid hcl 36%

 

[Polka999]

even if lines split after finishing adding HCL you should be good to go. they will still crystalize inside fridge (at least for me they crystalized)

 

[G.Patton]

Hello, yes, it is okay.

 

[GeneralX]

Greetings all! I can not understand the cause of black sediment at the bottom of the flask.

Here are my proportions for 500 grams of a-pvp

1. Bromvaleraphenone - 730 grams

2. ethyl acetate - 1600 ml.

3. Pyrollyddin - 360 ml

After I fully pour in the pyrollyddin, and stop the stirrer, a black precipitate starts to build up at the bottom of the flask.

I always keep the reaction temperature at 40-50 degrees!

What can this be?

 

[GeneralX]

Next, I remove this black sludge through a separating funnel, and continue the process. And all is well, a-pvp comes out!

The big question is what is that sediment at the bottom?

 

[Polka999]

I think it happens when you use low quality 2-bvp but pvp will still crystalize (but yield will be lower)

When i switched to high quality 2-bvp (10ML should weight around 13 grams) this black liquid at bottom was gone.

hope this helps also i might be wrong so let's wait for experts

 

[Polka999]

i should also note that after washing it's normal to have darker liquid at bottom

 

[YenaneY]

Is it possible to distill off the EtOAc without a chiller pump?

 

[Polka999]

Just heat it up at around 70 celsius untill EA smell is gone. but to be honest there is no need to evaporate EA. it should crystalize without EA evaporation.