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

[Ukspice]

@William Dampier

Need help with measurements

Instead of using :Valerophenone
I will buy liquid : 2-Bromovalerophenone

If I want to use 1litre

2-Bromovalerophenone​

What is the reagents amount I will need per I litrre:


-Hydrobromic acid (HBr) 48%;?

-Hydrogen peroxide (H2O2) 35%;?

-Pyrrolidine (CAS 123-75-1);???

-Ethyl acetate ;???

-Sodium carbonate (Na2CO3) 20% aq solution;???

-Diethyl ether (Et2O) ????

-EtOH 50 ???

-Dibenzoyl-D-tartaric acid ??

-Dichloromethane (CH2Cl2) 830 mL;

-Hexane ????

Hydrochloric acid conc. 35% (HCl);.??

WOULD REALLY HELP IF YOU CAN GET ME MEASUREMENTS FOR USE OF 1 LITRE 2-BROM. PLEASE?????

So that I can cost per reaction, also is the yield estimate about 20% loss
1 litre = 800g a-pvp?

 

[Marvin "Popcorn" Sutton]

I wrote you a PM.

 

[Spikkel93]

Got the same question can u send me also in pm ?
Thanks in advance

 

[GeneralX]

But despite this, I further continued to acidify with 37% hydrochloric acid, having previously added 30 ml of cold acetone. But still nothing formed, so far I put it in the freezer, but I feel that nothing will form. ph always shows around 5. Please help me

Spoiler: photo

 

[G.Patton]

You had to evaporate EA after the reaction. It interferes to form a-PVP HCl crystals.

 

[Bitwise]

if anyone can tell me if my thoughts are correct?can i just boil EA off at 1 atm?
for the boiling point of EA is like 77°C and the boiling point of a-pvp freebase is around 102°C, and the pyrrolidine boils at 87°C, if i controls the tempreture at about 100°C (for example add a little bit of water) and i will know when the liquid stops releasing the fog that smells like ammonia then add some well calculated amount of HCL(aq),then boil the liquid left there, and there should be some wet mixture substance left in the bottom.
and then i will have something left in the beaker, which seemed to be mostly a-pvp hcl, little pyrrolidine hcl, some unreacted bromvaleraphenone, little water mixuture. treat it with acetone and put it in the refrigerator, then collect the powder, which seems to be a-pvp hcl. will it work?

 

[G.Patton]

Hi, for a what reason do you assume to add water there? Yes, you can heat the solution to 100*C but take into account that it's not okay for free base. It also will be evaporated partly. It's worth to use vacuum distillation!

 

[Bitwise]

vacuum distillation seem to bit a little .... expensive to me.
sadly i just cant afford them...

 

[SpaceRocket]

hello, I have a question, I have all the steps. followed the process and have a nice a-pvp with a result of 80%. I do it on a larger scale between 1 and 0.5 kg bromo, but now I wonder how I can get large, beautiful crystals because if I try to recrystallize in water it grows. back like little needles. You can see on the picturen powder what i have made and the cristals sombody els but he dont want to tel me how he did it if sombody can help me wild be great!!!

 

[G.Patton]

Hi, how do u recrystallize it?

 

[SpaceRocket]

I am loking for method how to cristalize , when i want to cristalize i get nedel cristal like this on the photo

 

[G.Patton]

a-PVP crystallization

 

[RegulierTier]

Can I replace the ethylacetate with toluene or TBME?
I don't have a rotovap so destill under vacuum would be a problem...

 

[SpaceRocket]

I did it with 2 infrared lamps and had to evaporate 16.9 ethiel acetate in plastic containers, which took me 30 hours and i dry my powder also with the lamps that go very fast in view hours your powder is dry

 

[W Alchemy wite]

Which precursors are needed for A-PiHP
Is the process the same?

 

[HIGGS BOSSON]

α-bromo-isohexanophenone, synthesis same a_PVP

 

[Newbee]

What other solvents can be used to replace ethyl acetate in amination stage ? What About DCM?
do procedure time change?
i want eliminate destilation step so preferably solvent that can be easily separated by funnel.

 

[NinjaFlakkaZombie]

Anyone know of a way I can get a free starters kit as this is my first synth and whatever I don't have to sink my entire paycheck into would be greatly appreciated. I have no problem giving up 99% of the yeild as payment

 

[Bitwise]

there is no short cuts if you want to do synth yourself
do as what the video told you to do and you will get the product

 

[SpaceRocket]

does anyone know how to make MDPHP? Or is it same like A-PVP?

 

[loadingST]

Yes theoreticaly i can help but md group is more hardly handled in FC, so maybe the more easier way is to make the ketone via grignard, and once you got the desired ketone, you can make whatever you want/the same as a-pvp.