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

[WillD]

3l of pyrrolidine for 1kg bromo should be ok?

JamrozNo. 0,9kg (~1L) of pyrrolidine for 1kg alpha-bromovalrophenone.

 

[FishAndChips]

No. 0,9kg (~1L) of pyrrolidine for 1kg alpha-bromovalrophenone.

William DampierYou mean the porpotion is 1L of Pyrrolidine for 1kg
2-bromovalerophenone but how many Ethyl acetate do l need to make Alpha-PVP?

 

[Frit Buchner]

You mean the porpotion is 1L of Pyrrolidine for 1kg
2-bromovalerophenone but how many Ethyl acetate do l need to make Alpha-PVP?

FishAndChips2.64848L per kg based on mole density
Mole of 2-b-v=242 grams
Mole of e acetate= 98ml

 

[Frit Buchner]

2.64848L per kg based on mole density
Mole of 2-b-v=242 grams
Mole of e acetate= 98ml

Frit BuchnerThat related to the 4L to 1.5 kg in the list

 

[madmoney69]

I have problems getting it crystalize. What common solutions is for it why I am having problems with getting crystals?

 

[🍒cherry]

I have problems getting it crystalize. What common solutions is for it why I am having problems with getting crystals?

madmoney69I think you must freeze the liquid for 2 days then u can see some crystal forming same like hmtd crystal synthesis not sure it might help
is more important in freezer crystallization

 

[G.Patton]

of hydrohloric acid (not to over-acidify the solution)?

komkomYou can use equimolar proportion and check pH of the solution.

12. Hydrochloric acid is added to pH 5.

 

[viking1111]

You can use equimolar proportion and check pH of the solution.

G.PattonSo if i have for example 80l freebase in EA after washing with water, how many l aceton should i use.

 

[komkom]

and how i can get mdpv instead of a-pvp?

 

[Frit Buchner]

and how i can get mdpv instead of a-pvp?

komkomI'm sputballing here and I'm not a chemist, but I'm guessing you start with 2-bromo-3,4-methylenedioxy benzene, react it with velaryl chloride to get 3,4-MD-valeraphenone

 

[a.hatam]

What could i replace Valerophenone with?

 

[Cranston]

I think you need Valerophenone for Alpha-PVP and Hexanophenone for Alpha-PHP.
Anybody knows the name of the base chemical for Alpha-PiHP?

 

[Cranston]

I think you need Valerophenone for Alpha-PVP and Hexanophenone for Alpha-PHP.
Anybody knows the name of the base chemical for Alpha-PiHP?

AlphaPipeIt's

Isohexanophenone​

or other name being

4-methylpentanophenone​

 

[Cranston]

I think you need Valerophenone for Alpha-PVP and Hexanophenone for Alpha-PHP.
Anybody knows the name of the base chemical for Alpha-PiHP?

AlphaPipeOf course, even of more interest is the next chemical in the process:

2-bromo-4-methylpentanophenone​

Any one knows a provider for it?

 

[komkom]

After water added at halogenation stage, i have that...
My questions:

1. What i do wrong?
2. It must be dropped out, or i can "save" expensive valphen (#1009...)?

thnx!

p.s. i'am mixing in hands, because my magnet stirrer can't mix it properly (small quantity of liquids)
but,,,, colors, bleaching and other things, are same as in video....

 

[Cranston]

After water added at halogenation stage, i have that...
My questions:

1. What i do wrong?
2. It must be dropped out, or i can "save" expensive valphen (#1009...)?

thnx!

p.s. i'am mixing in hands, because my magnet stirrer can't mix it properly (small quantity of liquids)
but,,,, colors, bleaching and other things, are same as in video....

komkomWhy aren't you using directly 2-Bromovalerophenone?
It looks easier to get than Pyrrolidine.

 

[viking1111]

Hello i have little problem, for 25k 2bromovalero i use to crysyalization after pirolidyne and after washing, i use to crystalization 1,5l aceton to 0,38 acid per 1kg bromo, but liquid to crystalization i take 1l and make ph 2 with mixture of aceton and acid, after 10h in freezer nothing happend (it was mixing 4 hours with pirolidyne on temp 55) what i did wrong and how to fix it?

 

[Marvin "Popcorn" Sutton]

Hello i have little problem, for 25k 2bromovalero i use to crysyalization after pirolidyne and after washing, i use to crystalization 1,5l aceton to 0,38 acid per 1kg bromo, but liquid to crystalization i take 1l and make ph 2 with mixture of aceton and acid, after 10h in freezer nothing happend (it was mixing 4 hours with pirolidyne on temp 55) what i did wrong and how to fix it?

viking1111I suggest we go to private messages and discuss the details with synthesis.

 

[pandachems]

anyone finally got the best finished apvp product ready now?

 

[viking1111]

What u mean

 

[Batracien]

Stage 2. Amination.

View attachment 1227

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α-PVP/MDPV synthesis from 2-Bromovalerophenone

• Novator
• Mar 23, 2023
• 90
• alpha-pvp cas 14530-33-7 flakka o-2387 synthesis video manual video tutorial α-pyrrolidinopentiophenone α-pyrrolidinovalerophenone β-keto-prolintane

α-PVP hydrochloride synthesis from 2-Bromovalerophenone (cas 49851-31-2)...

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1. Ethyl acetate 4 L is placed into a reactor with 2'-Bromovalerophenone 1.5 kg and stirred 5 minutes.
2. A drip funnel is installed at the reactor neck and pyrrolidine 1150 ml (CAS 123-75-1) is added into this funnel.
3. A drop funnel tap is opened and pyrrolidine is added dropwise with vigorous stirring.
4. The temperature is maintained below 65 ℃.
5. The reaction mixture is vigorously stirred for 1 hour after completion of the pyrrolidine addition.
8. A reactor vacuum pump and a chiller pump of reflux condenser are turned on.
9. The most part of ethyl acetate is distilled off.
10. A vacuum pump is stopped and acetone is added into the reactor. The stirring is continued.
11. Hydrochloric acid is added into the drip funnel on the reactor neck.
12. Hydrochloric acid is added to pH 5. A small amount of reaction mixture is drained from the bottom reactor tap to control pH with a litmus paper (also, you can use glass rod for this goal). The sample is returned to the reactor.
13. After that, the reaction mixture is poured into a beaker and put into a freezer for 12 hours.

William DampierHello, if I don't want to make a distillation is it a problem ? or is the distillation of the ethyl acetate just used to recover the solvent ? will it cause a problem with the a-pvp salt solubility ?

 

[grow111]

Can you use other solvent instead of ethyl acetate? Maybe IPA or xylene? Does it change results?

 

[G.Patton]

Can you use other solvent instead of ethyl acetate? Maybe IPA or xylene? Does it change results?

grow111Yes, benzene. It won't.

 

[komkom]

photo #1 2-bromovalerophenone with ethylacetate (my 2-b-vp is crystallized after halogenation may be it problem? but what i do wrong? maybe HBr is too concentraded? but after EtAc added it dissolved)
...
photo #2 decolorized and spoiled after 4-5 drops added of pyrrolidinen to Rm from Photo #1

Many thnx!