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

[Marvin "Popcorn" Sutton]

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.

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

spaggydeeit should have worked
what is the result?

 

[spaggydee]

it should have worked
what is the result?

Marvin Popcorn SuttonSorry for the late response. Life got in the way along with a few experiments consuming my time.


I've had a handful of few successful synths that had low yields, and I have a handful of synths that yielded nothing. I've saved all the 'mother liquor' from both successful and unsuccessful attempts.

Now I have like 2 gallons of this mother liquor, most of it is probably water and sodium salt and carbonate contamination.

Any tips on reducing and/or extracting out the intended product?

 

[pachemguy]

How much methylamine would one use for 1kg of bk ??

 

[OrgUnikum]

How much methylamine would one use for 1kg of bk ??

pachemguy262 g is absolute minimum, realistically 280 g - 300 g.
Thats 700 g - 750 g of a 40% MeNH2 solution in water, look at the 4-MMC synth which uses EtOAc for the workup/crystallisation as it won't work as here described for the water.

 

[OrgUnikum]

if use alkali, then half the amount of methylamine is needed in theory, then 1 mol of methylamine, 1 mol of bromovalerophenone and 1 mol of alkali. We also take into account that an aqueous solution of methylamine erodes during storage, a good excess of methylamine will additionally mix the reaction in the direction of the formation of aminoketone

w2x3f5Sure. I was going after the first post in the thread which does not mention alkali. The best alkali would be cesium carbonate, but potassium carbonate is known to work too, personally I would not use MeNH2 in water anyways, although a certain amount of water does not hurt, thats getting really a lot. I would use 1,2 equv. MeNH2.HCl and Triethylamine to free the methylamine from the salt and to scavenge the formed HBr.

I am also unsure how active the resulting compound is, I have the feeling the pyrovalerone might be superior. Any genuine knowledge regarding this question would be appreciated.

 

[w2x3f5]

Sure. I was going after the first post in the thread which does not mention alkali. The best alkali would be cesium carbonate, but potassium carbonate is known to work too, personally I would not use MeNH2 in water anyways, although a certain amount of water does not hurt, thats getting really a lot. I would use 1,2 equv. MeNH2.HCl and Triethylamine to free the methylamine from the salt and to scavenge the formed HBr.

I am also unsure how active the resulting compound is, I have the feeling the pyrovalerone might be superior. Any genuine knowledge regarding this question would be appreciated.

OrgUnikumwhy do you need cesium carbonate? )))))))))
all you have to do is bind the hydrobromic acid so it doesn't react with the methylamine...

 

[OrgUnikum]

why do you need cesium carbonate? )))))))))
all you have to do is bind the hydrobromic acid so it doesn't react with the methylamine...

w2x3f5Cesium is not essential but preferred, see the attached article.

 

[w2x3f5]

Cesium is not essential but preferred, see the attached article.

OrgUnikumwe are talking about aminoketone, in the patent just amine. Feel the difference?
the reaction is going well anyway, only alkali can be added to save the primary amine. alkali will only free the primary amine from the rest of the acid
yes, you forgot that amino ketones in a strongly alkaline environment are prone to the formation of piperazines, by analogy with mephedrone.

 

[OrgUnikum]

we are talking about aminoketone, in the patent just amine. Feel the difference?
the reaction is going well anyway, only alkali can be added to save the primary amine. alkali will only free the primary amine from the rest of the acid
yes, you forgot that amino ketones in a strongly alkaline environment are prone to the formation of piperazines, by analogy with mephedrone.

w2x3f5Sn2 Substitution on a bromoketone, sure. What patent are you talking about? I did not mention any patent.
The whole soup is strongly alkaline in any case, the substitution would not work with the salt of an amine. For scavenging of the formed HBr triethylamine can be used, also for converting MeNH2.HCl to the base without generating water.

I am not aware about the piperazine formation, could you point me somewhere where this is mentioned, some references would be great.

One might consider to add a small amount of NaI to catalyze the Sn2 when doing it in protic solvents or the presence of water.

An interesting question is of course if and if yes in what amount the formation of the hydroxyimine is taking place and if not a simple heating of the organic products in a suited solvent would rearrange this imine to the wanted aminoketone.

 

[w2x3f5]

Sn2 Substitution on a bromoketone, sure. What patent are you talking about? I did not mention any patent.
The whole soup is strongly alkaline in any case, the substitution would not work with the salt of an amine. For scavenging of the formed HBr triethylamine can be used, also for converting MeNH2.HCl to the base without generating water.

I am not aware about the piperazine formation, could you point me somewhere where this is mentioned, some references would be great.

One might consider to add a small amount of NaI to catalyze the Sn2 when doing it in protic solvents or the presence of water.

An interesting question is of course if and if yes in what amount the formation of the hydroxyimine is taking place and if not a simple heating of the organic products in a suited solvent would rearrange this imine to the wanted aminoketone.

OrgUnikumby analogy with the reaction with mephedrone, alkali catalyzes the formation of piperazines. there is no time to search, a cursory search shows the condensation reaction of alpha-aminoketone to piperazine in a strongly alkaline reaction (yes, not quite what you need, but plus or minus is similar).
Yes, that's right, not a patent, I didn't notice. In any case, if you install the synthesis, let me know about the results

 

[pachemguy]

by analogy with the reaction with mephedrone, alkali catalyzes the formation of piperazines. there is no time to search, a cursory search shows the condensation reaction of alpha-aminoketone to piperazine in a strongly alkaline reaction (yes, not quite what you need, but plus or minus is similar).
Yes, that's right, not a patent, I didn't notice. In any case, if you install the synthesis, let me know about the results

w2x3f5Thanks everyone gonna try to synth pyrrolidine direct from l-proline and copper carbonate I just have this 55gal drum of 40% laying around one day she find a good use

 

[VamonosPest]

Possible to use Xylene instead of Ethyl acetate?

 

[Undercoverfedboy]

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.​

View attachment 1228 ​

Equipment and glassware: View attachment 6933 ​

• 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.

View attachment 1226

Download Video

2-Bromovalerophenone synthesis from valerophenone

• Novator
• Jun 27, 2022
• 1
• 2-bromovalerophenone a-pvp cas 1009-14-9 cas 49851-31-2 methcathinones synthesis valerophenone video manual video tutorial α-pyrrolidinovalerophenone

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.

William DampierI have a couple questions about this process. In the video step 13 and 15 are skipped? Do you add sodium hydroxide to the solution and in what amount? I attempted the procedure last night and the water fell to the bottom. Any help would be greatly appreciated! Edit: the halogenation step is the one in question.

 

[fuctupkornfan]

How easy would this be for domaine with little to no backgrounf in chemistry? Also what would the budget for sourcing all the material be?

 

[Marvin "Popcorn" Sutton]

How easy would this be for domaine with little to no backgrounf in chemistry? Also what would the budget for sourcing all the material be?

fuctupkornfanIf you're serious about it, then write me or another expert in the personal area and we'll tell you everything. The synthesis of a-pvp is one of the simplest.

 

[fuctupkornfan]

It certainly seems like the cheapest option and given how difficult finding this product is. It may be the easiest. I'm just curious as to what legal consesuences could be given its for prrsonal use?

 

[airsoft45]

does the bromination stage produce any actual bromine as a by product?

 

[Shehry]

Hi respected members, I have a question because of my little chemistry knowledge. please refer Stage 2. Amination, point 9, After distilling off Ethyl acetate acetone is added then HCl is added for crystallization of pvp.HCl salt. My question is if there is some un-reacted Pyrrolidine at this stage, it will also react with HCl and will be converted into water soluble salt as Pyrrolidine.HCl. Therefore it will be extremally difficult to get rid off this dangerous and unwanted chemical. Why not reaction mixture is washed with water after complete mixing of Pyrrolidine and prior to distilling of Ethyl acetate to get rid off any un-reacted Pyrrolidine. I am sure my apprehension will be wrong, but how...? please teach me for my own satisfaction. Wishing good luck to all.

 

[Marvin "Popcorn" Sutton]

Hi respected members, I have a question because of my little chemistry knowledge. please refer Stage 2. Amination, point 9, After distilling off Ethyl acetate acetone is added then HCl is added for crystallization of pvp.HCl salt. My question is if there is some un-reacted Pyrrolidine at this stage, it will also react with HCl and will be converted into water soluble salt as Pyrrolidine.HCl. Therefore it will be extremally difficult to get rid off this dangerous and unwanted chemical. Why not reaction mixture is washed with water after complete mixing of Pyrrolidine and prior to distilling of Ethyl acetate to get rid off any un-reacted Pyrrolidine. I am sure my apprehension will be wrong, but how...? please teach me for my own satisfaction. Wishing good luck to all.

ShehryIn this synthesis it is assumed that the pyrrolidine residue will volatilize when distilled with ethyl acetate. If not distilled off, it can be washed with water.

 

[Ukspice]

MONKEY DUST - MDPV

Is it the same as a-PVP?

What is the difference when trying to synthesis MDPV?...

 

[Ukspice]

I have been told to make:
MONKEY DUST - MDPHP/MDPV

It is the same process as making a-pvp

But use this reagent instead:
CAS No. 63740-98-7
1-(Benzo[d][1,3]dioxol-5-yl)pentan-1-one

THE QUESTION is which chemical is replaced in the process??????

which one: Valerophenone (CAS 1009-14-9) Or 2-Bromovalerophenone
is Swapped with:
1-(Benzo[d][1,3]dioxol-5-yl)pentan-1-one

To make the monkey dust ?????

 

[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]

@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?

UkspiceI wrote you a PM.

 

[Robertos]

I wrote you a PM.

Marvin "Popcorn" Suttonhi,i have the same question , can you ableto help?