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



## William Dampier (Jul 21, 2021)

*Introduction*
This topic is represented alpha-PVP synthesis way in a medium scale 1-10 kg. There are elaborated video tutorials, which are allowed to produce this substance to anybody. Also, you can find here a list of necessary equipment and reagents.​


​*Equipment and* *glassware**:

*​
Round bottom flask;
Retort stand and clamp for securing apparatus;
Reflux condenser;
Drip funnel;
pH indicator papers;
Beakers;
Vacuum source;
Laboratory scale (1-2000 g is suitable);
Measuring cylinders 100, 500 and 1000 mL;
Top stirrer with heating plate;
Glass rod and spatula;
Separatory funnel 1 L ;
Laboratory grade thermometer; 
Buchner flask and funnel; 
Vacuum source;
Filter paper;
Rotary evaporator;
Conventional funnel;

*Reagents:*​
Valerophenone (CAS 1009-14-9) 1 kg;​
Hydrobromic acid (HBr) 290 ml 48%;​
Hydrogen peroxide (H2O2) 190 ml 35%;​
Pyrrolidine 1100 ml (CAS 123-75-1);​
Ethyl acetate 4 L;​
Sodium carbonate (Na2CO3) 20% aq solution;​
Diethyl ether (Et2O) 50 ml;​
EtOH 50 mL;​
Dibenzoyl-D-tartaric acid 12.7 g, 35.5 mmol;​
Dichloromethane (CH2Cl2) 830 mL;​
Hexane 1100 mL;​
Hydrochloric acid conc. 35% (HCl);​
​*Stage 1. Halogenation.*













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2-Bromovalerophenone synthesis from valerophenone



__ Novator
__ Jun 27, 2022
__
2-bromovalerophenone
a-pvp
cas 1009-14-9
cas 49851-31-2
methcathinones
synthesis
valerophenone
video manual
video tutorial




Valerophenone halogenation (CAS 1009-14-9) to 2-Bromovalerophenone (CAS 49851-31-2)...




​1. Valerophenone (CAS 1009-14-9) 1 kg is weighed and poured into the reactor.
2. Hydrobromic acid (HBr) 290 ml 48% is added.
3. The reaction mixture is stirred vigorously for 5 minutes.
4. Hydrogen peroxide (H2O2) 190 ml 35% is added into the drip funnel and installed onto the reactor neck.
5. A drop funnel tap is opened and hydrogen peroxide is added dropwise with vigorous stirring.
6. Look at the color of the mixture. Color may vary from yellow to red. Hydrogen peroxide is added so that mixture is discolored.
7. The temperature is maintained below 65 ℃. The H2O2 dripping is stopped in case the temperature is risen.
8. Step *2-7* are repeated twice after the complete hydrogen peroxide addition
9. The reaction mixture is vigorously stirred for 1.5-12 hours.
10. Distilled water is added and the reaction mixture is stirred for 5 minutes.
11. The stirring is stopped and the reaction mixture is separated into two layers. The target layer is on the bottom, water is on the top layer.
12. The water layer is removed with help of a vacuum pump through the reactor neck.
13. An aqueous alkaline solution is added and stirred for 5 minutes.
15. Step *10*,* 11*,* 12* are repeated.
16. The resulting product is left in the reactor.

*Stage 2. Amination.*
*












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α-PVP/MDPV synthesis from 2-Bromovalerophenone



 Novator
 Jun 23, 2022
 11

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)...




*​1. Ethyl acetate 4 L is placed into a reactor and stirred 5 minutes.
2. A drip funnel is installed at the reactor neck and pyrrolidine 1100 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.

*Stage 3. Filtration.*
1. A vacuum filtration system is installed (nutsche filter, filter cloth, vacuum pump).
2. A vacuum pump is turned on.
3. The reaction mixture is poured from the beaker (from step *13* stage *2*) to Buchner funnel.
4. The reaction mixture is filtered and pressed until a solid is obtained.
5. A cold acetone is poured into Buchner funnel to cover the whole solid.
6. Acetone is filtered and product is washed. Step *5* is repeated in case the solid substance is not white.
7. The content of Buchner funnel is poured into the Pyrex dish for drying procedure after the acetone filtration and the white solid obtaining.
8. The Pyrex dish is placed in a dry place at room temperature.
9. The product is dried to constant mass. Product is mixed and crushed periodically in order to rise drying speed.

*Stage 4. Diastereomeric.*


​1. a-PVP HCl 10.0 g, 35.5 mmol is dissolved in minimum volume of distilled water .
2. Na2CO3 20% aq solution is added to reach pH 8-9.
3. The mixture is extracted with Et2O 50 ml.
4. Ether extract is separated in a separatory funnel, then Et2O is distilled off.
5. a-PVP free base is dissolved in EtOH (50 ml).
6. Ethanol solution of a-PVP free base is heated to 70 ℃.
7. Dibenzoyl-D-tartaric acid 12.7 g, 35.5 mmol is added.
8. The solution is refluxed with a reflux condenser for 1 minute and cooled to a room temperature.
9. A solvent is distilled off.
10. The residue is dissolved in CH2Cl2 (530 mL). Hexane (700 mL) is added with stirring.
11. The resulting crystals (9.1 g) are collected by filtration through a Buchner flask and funnel after 3 days.
12. Three consecutive recrystallizations from CH2Cl2/hexane (300/400 mL) are given a single diastereoisomer (6.1 g, 61%);
13. Steps *1*, *2*, *3* are repeated with salt from step *11*.
14. A cold acetone is added.
15. Hydrochloric acid (HCl) is added to reach pH 5.
16. Pruduced crystals from step *15* are filtered and air dried.


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## BHBlueberry

Very precise recipe  Thank you. Could you analyse the Hex-en recipe?


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## ASheSChem

Pyrrolidine is findable in Europe ?


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## Morpheus77

Would love to take a shot at this. Wondering if Cu(II)Br could be used for halogenation rather than HBr though


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## Jamroz

can you give the proportions for the amination for 1kg 2-bromovalerophenone ?
​


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## William Dampier

Jamroz said:


> can you give the proportions for the amination for 1kg 2-bromovalerophenone ?



Jamroz2-3 equal molarity to bromoketone for selected amine


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## Jamroz

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


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## William Dampier

Jamroz said:


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



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


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## baxter192

where i can find a vendor for pyrrolidin?


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## G.Patton

baxter192 said:


> where i can find a vendor for pyrrolidin?



baxter192You can search at Listing or use another souses.


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## The Silent Chemist

Can N-METHYL-2-PYRROLIDONE be used


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## G.Patton

The Silent Chemist said:


> Can N-METHYL-2-PYRROLIDONE be used



The Silent Chemistno


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## madmoney69

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


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## komkom

Hydrochloric acid 20% can be used? (or need >=35%)?
Or, instead of hCl, can be used 1,4-Dioxane (CAS: 123-91-1)? or dioxane hydrochloric acid (20%) ?


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## G.Patton

komkom said:


> Hydrochloric acid 20% can be used? (or need >=35%)?



komkomYes, it can be used


komkom said:


> can be used 1,4-Dioxane (CAS: 123-91-1)?


no, it won't form hydrochloride salt with a-PVP


komkom said:


> or dioxane hydrochloric acid (20%) ?


Do you mean hydrochloric acid 20% dioxane solution? I think yes.


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## madmoney69

Finally my A-PVP synthesis was success.
I had problems to crystalize it and had difficulty to understand what was my mistakes.
But what was needed is to evaporate most of EA, add cold acetone 1:1 and after added enough HCL it started crystalizing almost imediatly.
THNX to the BBgate experts, especially for G.Patton


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## Didi

madmoney69 said:


> Finally my A-PVP synthesis was success.
> I had problems to crystalize it and had difficulty to understand what was my mistakes.
> But what was needed is to evaporate most of EA, add cold acetone 1:1 and after added enough HCL it started crystalizing almost imediatly.
> THNX to the BBgate experts, especially for G.PattonView attachment 8118View attachment 8119



madmoney69


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## Didi

How much u get gram ??


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## spaggydee

madmoney69 said:


> Finally my A-PVP synthesis was success.
> I had problems to crystalize it and had difficulty to understand what was my mistakes.
> But what was needed is to evaporate most of EA, add cold acetone 1:1 and after added enough HCL it started crystalizing almost imediatly.
> THNX to the BBgate experts, especially for G.PattonView attachment 8118View attachment 8119



madmoney69I've run into a similar issue a few times - so I appreciate your insight on what solved your issue.

Luckily, somehow, my first synth was smooth sailing and error free - but strangely since then it seems that every other one I've done has weird issues with crystallizing small yields and/or mainly being an oil. I'm not sure where my error is because when I do another synth, it then seems to be successful.

My last synth, for example, is behaving in a way I've never seen before - it crystallizes with heat/air applied and assisted with acetone, however when removed from heat it slowly liquifies back into an oil.

Fingers crossed that my next run doesn't waste further material.


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## madmoney69

If you still have that material. Try to evaporate all excess solvent add acetone 1:1 cool down all and add more HCL until starts forming crystals.


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## madmoney69 (Nov 29, 2022)

Less than I should. But there is room for improvement



Didi said:


> How much u get gram ??



Didi


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## spaggydee

madmoney69 said:


> If you still have that material. Try to evaporate all excess solvent add acetone 1:1 cool down all and add more HCL until starts forming crystals.



madmoney69Will do and I'll report back the results. 

Hopefully I get something out of it because last night I actually attempted a small A/B extraction to see if that'd help clean it up, but ran out of sodium hydroxide midway. Local stores were closed, and me being impatient, I then used copious amounts of sodium carbonate to neutralize the remaining HCL from my material. 
Since then I've cleaned up most of the salty aqueous layer and still have the organic layer.

Long story short - I gave myself a lot of work for probably all the wrong reasons. Wish me luck!


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## komkom

1. In video, present: ~1 kilo (~700ml) of bromovalerophenone?
2. This proportions are correct? 100g(bk),110ml(pyrrolidine),400ml(EtAc),60ml(distilled water)?
3. In video u adding water at amination stage, but in forum text-message acetone added, what difference?


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## spaggydee

baxter192 said:


> where i can find a vendor for pyrrolidin?



baxter192Pyrrolidine can be prepared via decarboxylation of Proline by refluxing it using Acetophenone as a catalyst. 

There are also other publications of using other catalysts, but if you have access to acetophenone that is the simplest in my opinion. In terms of the process and cleanup.


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## Marvin "Popcorn" Sutton

spaggydee said:


> Will do and I'll report back the results.
> 
> Hopefully I get something out of it because last night I actually attempted a small A/B extraction to see if that'd help clean it up, but ran out of sodium hydroxide midway. Local stores were closed, and me being impatient, I then used copious amounts of sodium carbonate to neutralize the remaining HCL from my material.
> Since then I've cleaned up most of the salty aqueous layer and still have the organic layer.
> ...



spaggydeeit should have worked
what is the result?


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## Marvin "Popcorn" Sutton

komkom said:


> 1. In video, present: ~1 kilo (~700ml) of bromovalerophenone?
> 2. This proportions are correct? 100g(bk),110ml(pyrrolidine),400ml(EtAc),60ml(distilled water)?
> 3. In video u adding water at amination stage, but in forum text-message acetone added, what difference?



komkom
100g bk,100ml pyrrolidine (~90g) ,400ml EtAc
these are the correct proportions for the AMINATION step 
after completion of the reaction add 600ml of water to wash and separate the organic phase
acetone is added before acidification, after the organic layer has been separated from the aqueous layer.


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## madmoney69

If I get 50-60g a-pvp per 100g of 2-bromovalerophenone how I can increase yields?


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## sleeplessmania

madmoney69 said:


> If I get 50-60g a-pvp per 100g of 2-bromovalerophenone how I can increase yields?



madmoney69This question of yours is extremely non-specific, as in you never measured which part of the synthesis you notice loss in total yield.

Also, let's not forget that if you want clean, alpha of the alpha-pvp's you will have to no matter what purify & crystallize & then re-crystallize till you start pulling your own hair out of anger, to the point where the alpha-pvp is at a level that will satisfy your or your clients needs, as depending on their road of administration, if the product is not clean enough they will be angerful about the taste if vaporized, the causticity if intraveniously administered, or insufflated.

Applying the upper mentioned, try to make some calculations and note them down too with each step in your procedure, then try to see if there is any problems, and don't forget to purify it.


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## Germanium

If you want to make α-PHP, do you replace valerophenone with hexanophenone and follow the same method?


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## G.Patton

Germanium said:


> If you want to make α-PHP, do you replace valerophenone with hexanophenone and follow the same method?



GermaniumYes, correct.


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## Germanium

G.Patton said:


> Yes, correct.



G.PattonThank you!


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## komkom

hmmm, how i can calculate acetone size (ml) (crystalization stage, after water layer was removed) and (~ ml) of hydrohloric acid (not to over-acidify the solution)?


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## G.Patton

komkom said:


> 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. *


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## danim18

guys this reagents is for how many gr a-pvp ? 
*Reagents:*

Valerophenone (CAS 1009-14-9) 1 kg;
Hydrobromic acid (HBr) 290 ml 48%;
Hydrogen peroxide (H2O2) 190 ml 35%;
Pyrrolidine 1100 ml (CAS 123-75-1);
Ethyl acetate 4 L;
Sodium carbonate (Na2CO3) 20% aq solution;
Diethyl ether (Et2O) 50 ml;
EtOH 50 mL;
Dibenzoyl-D-tartaric acid 12.7 g, 35.5 mmol;
Dichloromethane (CH2Cl2) 830 mL;
Hexane 1100 mL;
Hydrochloric acid conc. 35% (HCl);


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## G.Patton

danim18 said:


> guys this reagents is for how many gr a-pvp ?
> *Reagents:*
> 
> Valerophenone (CAS 1009-14-9) 1 kg;
> ...



danim18The yield is quantitative, around 100%.


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## Novator

madmoney69 said:


> But what was needed is to evaporate most of EA, add cold acetone 1:1 and after added enough HCL it started crystalizing almost imediatly.



madmoney69It is advisable to always evaporate extractants from a freebase before the crystallization stage.


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## bdog21

so in the first part, synthesizing 2-bromovalerophenone from valerophenone, approx how much 2-bromo will that yeild? im wondering because if one were to just start by buying 2-bromovalerophenone and skip that step how much would one need to fit into the rest of the proportions etc? and about how much a-pvp in the end will the specified amounts yield?


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## G.Patton

bdog21 said:


> so in the first part, synthesizing 2-bromovalerophenone from valerophenone, approx how much 2-bromo will that yeild? im wondering because if one were to just start by buying 2-bromovalerophenone and skip that step how much would one need to fit into the rest of the proportions etc? and about how much a-pvp in the end will the specified amounts yield?



bdog21Hello, as I wrote in my previous mesage, the yield is quantitative. It means that from each 1 mole Valerophenone you'll get 1 mole 2-bromovalerofenon. Read more about moles, grams, litres and chemical calculations here.


G.Patton said:


> The yield is quantitative, around 100%.


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## Hank Schrader (Monday at 11:15 PM)

My team is the largest in the CIS countries for the production of such things as salt.
Our main product in cathinones is A-PVP hydrochloride.
Our production technology allows us to complete the entire cycle from start to finish. 
All precursors that are practically used are produced by our team.
Bromination is carried out on an industrial scale with the absorption of hydrobromic acid.
The brominated ketone is neutralized and replaced by pyrrolidine.
Then there is the stage of obtaining salt and crystallization.
My product has excellent organoleptic properties and high purity.
We are the power of the chemical industry.
Ready to cooperate with manufacturers and wholesalers.
With us, you can learn how to brominate on an industrial scale or already use ready-made brominated ketones. Increase your production volumes hundreds of times!
Start cooperating with us, 
we are the best team from the CIS.


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## StarWars (Monday at 11:15 PM)

Hank Schrader said:


> My team is the largest in the CIS countries for the production of such things as salt.
> Our main product in cathinones is A-PVP hydrochloride.
> Our production technology allows us to complete the entire cycle from start to finish.
> All precursors that are practically used are produced by our team.
> ...



Hank SchraderWhat IT is ??


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## VamonosPest

What could i replace pyrrolidine with?


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## Hank Schrader

VamonosPest said:


> What could i replace pyrrolidine with?



VamonosPestMethylamine. You will get also good product.


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## G.Patton

VamonosPest said:


> And how about the legality of pyrrolidine and 2-bromovalerophenone?
> are these watched in europe can i order them safely?



VamonosPestHi. They are legal in EU.


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## VamonosPest

G.Patton said:


> Hi. They are legal in EU.



G.PattonThank you for reply


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## Hank Schrader (Monday at 11:15 PM)

My team is the largest in the CIS countries for the production of such things as salt.
Our main product in cathinones is A-PVP hydrochloride.
Our production technology allows us to complete the entire cycle from start to finish. 
All precursors that are practically used are produced by our team.
Bromination is carried out on an industrial scale with the absorption of hydrobromic acid.
The brominated ketone is neutralized and replaced by pyrrolidine.
Then there is the stage of obtaining salt and crystallization.
My product has excellent organoleptic properties and high purity.
We are the power of the chemical industry.
Ready to cooperate with manufacturers and wholesalers.
With us, you can learn how to brominate on an industrial scale or already use ready-made brominated ketones. Increase your production volumes hundreds of times!
Start cooperating with us, 
we are the best team from the CIS.


----------



## StarWars (Monday at 11:15 PM)

Hank Schrader said:


> My team is the largest in the CIS countries for the production of such things as salt.
> Our main product in cathinones is A-PVP hydrochloride.
> Our production technology allows us to complete the entire cycle from start to finish.
> All precursors that are practically used are produced by our team.
> ...



Hank SchraderWhat IT is ??


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## VamonosPest

What could i replace pyrrolidine with?


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## Hank Schrader

VamonosPest said:


> What could i replace pyrrolidine with?



VamonosPestMethylamine. You will get also good product.


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## VamonosPest

Hank Schrader said:


> Methylamine. You will get also good product.



Hank SchraderAnd how about the legality of pyrrolidine and 2-bromovalerophenone? 
are these watched in europe can i order them safely?


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## G.Patton

VamonosPest said:


> And how about the legality of pyrrolidine and 2-bromovalerophenone?
> are these watched in europe can i order them safely?



VamonosPestHi. They are legal in EU.


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## VamonosPest

G.Patton said:


> Hi. They are legal in EU.



G.PattonThank you for reply


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## madmoney69

Have pyrrolidine 4kg left if smb need. Only europe


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