Yield

[Apvp-amateur]

I started with 400grams of valerophenone in a 3 neck roundbottom..
Added 430gram of hbr48 while stirring
Put 172 gr of hydrogen peroxide 35% in the drip funnel.. periodically added a small stream until color became red, keeping temp below 65 degree celsius.. the last bit of peroxide made the solution in the roundbottom dark red and it stayed red even after langer time of mixing .. added 1.5 liter water let it mix for 10 minutes .. put the solution in a separator funnel and took the bottom part .. the weight of the produced 2-Bromovalerophenone was 460gram

I poured the 2-Bromovalerophenone in the roundbottom followed by 2liter ethyl acetate and started mixing..
in the drip funnel i put 410gr of Pyrrolidine.

Over a period of 2 hour while vigourously stirring i add the Pyrrolidine drop by drop.. afterwards 1.5 liter water was added and the solution was put in the separator funnel again .. i took the top layer from the funnel and put it in a beaker .. added 2.1 liter cold acetone.. and put hydrocloric acid 30% inside while mixing until ph is 5..
Afterwards i place the beaker in the freezer and leave it for 12 hours.

After retrieving of the product and cleaning with acetone i maybe have 250gr of a-pvp ..(way too little if you ask me).



I did the same procedure again with the same amounts .. only difference was in step1: the color did not become dark red and stayed red.. so i added more peroxide trying to get to the red color point.. the normal color of 2-Bromovalerophenone is kinda off white milky , this time i had dark red 2-Bromovalerophenone.. the rest of the reactions went the same only the color was off .. but then when i was putting in the hydrocloric acid , i could already see it starting to crystallis and all of the sudden …

The entire 5 liter beaker was solid with crystals and like minimal double the amount came of a-pvp came out ..



The normal batch i produced a couple of times and everybodt says it is the Bomb.. i have not yet tested this big yielding result yet .. can someone explain what i am doing wrong and therefor have such a small yield..

 

[loadingST]

The red color is indicating over bromination(unreacted bromine), therefore afther pyrrolidine addition is copmpleted, stir for some hours more, better learn to prepare a TLC, so you can check periodicaly when your precursor is consumed and transformed entirely.

 

[Apvp-amateur]

I was hoping for comments that would point me in the Right direction with my measurements for each chemical. Or Where i obviously did something incorrect

 

[loadingST]

Im not much into details with this synthesis, i think you just didnt leave it to react enough the first time, or didnt use the right ratio, i cant know as i havent watching what you did, you can write anything actualy as you dont understand, and if there have been some free bromine in it, it may have reacted with the aromatic structure of the ketone and you might have some traces para-bromo-apvp, bromopyrrolidine.hcl and so on in it. Did you washed well the non polar phase ? Did you recrystalized you apvp ? I even recomend isomer separation for this drug, as levo apvp is much better drug.