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

[Marvin "Popcorn" Sutton]

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.

 

[dkemist15021982]

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.

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

 

[The Silent Chemist]

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

dkemist15021982You need to wash the free base carfully with water first to remove the pyrrolidine, after that then your standard recrystallisation from acetone or ethanol

 

[VamonosPest]

What could i replace pyrrolidine with?

 

[Hank Schrader]

What could i replace pyrrolidine with?

VamonosPestMethylamine. You will get also good product.

 

[G.Patton]

Of course there is no arguing in: "Chemical1 is not listed as illegal." The fact only that it can be used to produce an illegal drug is easily enough to get a full sentence. The good site about it is: When the people catch you, you will have a much worse fate.
I hear in other parts of the world, like Texas, there is about the same. Therefore this neglect here is not understandable.

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

 

[Caleb]

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

G.PattonActually 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.

 

[The Silent Chemist]

Hey all any help would be much appreciated, I had my first attempt at the apvp synthesis today.

During stage 1 halogenation, I followed the procedure excatctly as the video discribes adding the H202 slowly to the reaction vessel that contains the valerophenone and hydrobromic acid, ensuring the temperature did not exceed 60c.

I noticed that the red bromine colour persisted and did not go away after adding 2/3rds of the 43g of H202. I took this as my visual cue to not add any more peroxide.

(I assumed this was because I concentrated my peroxide from 6% to the 37% via boiling off the water under vacuum and I may have over concentrated it a little)

I let the reaction mixture stir for 10mins to ensure that the red colour would not go away. It did not.

shortly after adding 500ml of distilled water to the reaction the bottom bromovalerophenon layer turned from red to milky white.

my guess is I did not add enough peroxide and let the reaction stir long enough. I have discarded it and will try again.

any help would be appreciated

 

[The Silent Chemist]

Hey all any help would be much appreciated, I had my first attempt at the apvp synthesis today.

During stage 1 halogenation, I followed the procedure excatctly as the video discribes adding the H202 slowly to the reaction vessel that contains the valerophenone and hydrobromic acid, ensuring the temperature did not exceed 60c.

I noticed that the red bromine colour persisted and did not go away after adding 2/3rds of the 43g of H202. I took this as my visual cue to not add any more peroxide.

(I assumed this was because I concentrated my peroxide from 6% to the 37% via boiling off the water under vacuum and I may have over concentrated it a little)

I let the reaction mixture stir for 10mins to ensure that the red colour would not go away. It did not.

shortly after adding 500ml of distilled water to the reaction the bottom bromovalerophenon layer turned from red to milky white.

my guess is I did not add enough peroxide and let the reaction stir long enough. I have discarded it and will try again.

any help would be appreciated

The Silent ChemistThe distilled water I used was contaminated with Hcl, litmus test showed it was acidic. A second run has now been attempted with no problems with the addition of water, the reaction stay dark red upon first wash with distilled water, a second wash was done with an alkaline solution as what the written instructions request, this second wash did lighten bromovalerphenone colour to a golden yellow.

 

[islandgato]

A-PHP synthesis would be awesome !

 

[ChemKing]

4-bromo-Alfa-pvp.
He carried out the synthesis of this substance. But I ran into a problem - it is very poorly soluble in water. What could be the reason? Synthesis began with 4-brimvalerophenone. He performed bromination, received 4-bromo-alpha-bromvalerophenone. Then he carried out a reaction with pyrrolidine. Then I got the salt using HCl. The final product is very poorly soluble in water. About 10g per 100ml

 

[Batracien]

Hello, I have done the bromination and the amination step but i'm not sure of the proportions I've used in the amination.
How much moles of pyrrolidine is needed for 1 mole of 2-bromovalerophenone, I used 2 moles pyrro for 1 mole bromovalerophenone, but here you all say that the good proprotions are : 100g bk (0.4mole) / 100ml pyrro (1.2mole) so 1/3.
Why it isn't possible to use 1/1 or 1/2, I don't understand why so much excess is needed. And EtOAc just act as a solvent or is the molar ratio of EtOAc important as well ?

 

[The Silent Chemist]

If you read carefully further back in the chat you will see the correct ratios stated, let me know how you go trying to crystallise the A-pvp. An excess is used to ensure all the bromvalerophenone is reacted. I am having difficulty getting it too precipitate out of solution. If you have trouble try distilling the free base under vacuum, ensure all solvents are anhydrous.

 

[Batracien]

If you read carefully further back in the chat you will see the correct ratios stated, let me know how you go trying to crystallise the A-pvp. An excess is used to ensure all the bromvalerophenone is reacted. I am having difficulty getting it too precipitate out of solution. If you have trouble try distilling the free base under vacuum, ensure all solvents are anhydrous.

The Silent ChemistI'm going to try evaporate EtOAc (and possible leftover pyrrolidine) in a water bath and OUTSIDE (I don't want to die), and dilute the free base with 0°C acetone (99%), then add hydrochloric acid (23%) until ph = 5 and finally put it in the freezer to filter it, do you think it will work ?

 

[Batracien]

I have an other problem concerning storage, I stored my 2-bromovalerophenone for almost 6months at normal conditions, and it seemed to have 0 effects on it. But what about my freebase/EtOAc, it was first slightly yellow, and now after a week it is orange, I have to store it because I Don't have time to go outside to my improvised forest laboratory for a month. Thank you for your advices and good luck !

 

[w2x3f5]

I have an other problem concerning storage, I stored my 2-bromovalerophenone for almost 6months at normal conditions, and it seemed to have 0 effects on it. But what about my freebase/EtOAc, it was first slightly yellow, and now after a week it is orange, I have to store it because I Don't have time to go outside to my improvised forest laboratory for a month. Thank you for your advices and good luck !

BatracienEvaporate ethylacetate and further fractionally evaporate the base in a vacuum.

 

[mb16]

In stage 4 diasteromeric. It says...

"1. a-PVP HCl 10.0 g, 35.5 mmol is dissolved in minimum volume of distilled water"

A-pvp has a molar mass of 231.33g wouldn't that make 35.5 mmol of a-pvp to be 82.12g and not 10.0g as stated above?

Also it seems a little overkill to use 700ml of hexane and 530ml of DCM to dissolve 10.0g of a-pvp.

Is this supposed to be starting from 100g and not 10.0g, is there a decimal in the wrong place here perhaps?

 

[mb16]

Sorry I mean...

A-pvp has a molar mass of 231.33g wouldn't that make 35.5 mmol of a-pvp to be 8.21g and not 10.0g as stated above?

 

[mb16]

No sorry the molar mass of a-pvp (HCl) is 267.8g which would make 35.5 mmol 9.5g.