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

[spaggydee]

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!

 

[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?

 

[spaggydee]

Pyrrolidine 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.

 

[Marvin "Popcorn" Sutton]

it should have worked
what is the result?

 

[spaggydee]

Sorry 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?

 

[Marvin "Popcorn" Sutton]

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.

 

[trump69]

What's bk?

 

[dkemist15021982]

Hi can somebody tell me how i can get rid off an harsh pyrrolidine tast that i have with.my selfmade pvp?

 

[The Silent Chemist]

You need to wash the free base carfully with water first to remove the pyrrolidine, after that then your standard recrystallisation from acetone or ethanol

 

[madmoney69]

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

 

[sleeplessmania]

This 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.

 

[Germanium]

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

 

[G.Patton]

Yes, correct.

 

[Germanium]

Thank you!

 

[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)?

 

[G.Patton]

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

 

[viking1111]

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

 

[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);

 

[G.Patton]

The yield is quantitative, around 100%.

 

[Novator]

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

 

[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?

 

[G.Patton]

Hello, 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.

 

[Hank Schrader]

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!
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[StarWars]

What IT is ??

 

[VamonosPest]

What could i replace pyrrolidine with?

 

[Hank Schrader]

Methylamine. You will get also good product.

 

[G.Patton]

You wrote quite obvious things. What is a main idea of your message?

 

[Caleb]

Actually the idea was to show (again) that people using substances are being treated llike criminals.
In some places they are even seen worse than child molesters and suicide bombers.
This speaks for itsel.