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Phenylacetone (P2P) synthesis from benzaldehyde with butanone

Fenster

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Ok, step 3 - I added NaOH solution heated to 50c and put into mag Stir after 6 hours a thick almost solid creamy mess was in my rbf. I added DCM and two layers appeared. At first, I was very happy!!! As the creamy thick layer sat on the bottom and I thought the clearer layer was the DCM extracted goodies was on top. No no no..... The Milky thick layer was the DCM. I know for a fact that when I remove the DCM I'm not going to have a yellow clear oil aka p2p.


@HEISENBERG

Have you team reviewed this process before publishing. Seems the experts have gone silent on this proceedures. Would be nice to get some support on a method your team published.

Ok, so I'll attempt Distillation on the creamy mess and see what comes over.
 

G.Patton

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I added DCM and two layers appeared.
You ask about method review but you don't follow the method and complaining that something went wrong :unsure:
2. Reaction solution is extracted with chloroform
DCM is non-polar solvent, chloroform is polar solvent.
 

Fenster

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D
You ask about method review but you don't follow the method and complaining that something went wrong :unsure:

DCM is non-polar solvent, chloroform is polar solvent.
DCM has a dipole moment. It is polar albeit slightly.

Are you sure your a chemist? I don't mean to be rude but DCM is not an NPS in the traditional sense.

Can I ask, have you or your team performed this method in totality?
 

Fenster

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What I need help with is the step 2.

I have 50% H2O2 and GAA. The amounts in the write up are 10L of GAA and 1300g of H2O2.

Are they expecting me to weigh the 50% H2O2 or am I supposed to accept it as a typo and use 1300ml?

The other write up is using sodium percarbonate directly and this write up here is generating it in situ. With GAA and H202.

I just need to confirm the amounts listed.
 

Fenster

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50% H2O2 = 1.197g/ml

1300g h202 (50%) = 1086ml

10:1 GAA to H2O2 to make acid in situ.

Is this the amount or is it a typo?

This process is being completed with lab grade reagents and glassware so if I follow it directly I should get the same results. However this write up needs work. Let's get this corrected and published as it should be.
 

Fenster

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2.2.4. 2-Acetoxy-1-phenyl-1-propene 4
Sodium perborate (5 g, 32 mmol) was added portion-wise over
6 h to a mixture of 3-methyl-4-phenyl-3-buten-2-one 3 (2 g,14 mmol), glacial acetic acid (7 mL, 0.122 mol), and acetone (4 mL)
at 55 8C. The solution was heated under reflux at 55 8C for a total of 24 h. Upon cooling to room temperature, water (20 mL) was added
followed by extraction with chloroform. The organic solution was dried (Na2SO4) and the solvent removed under vacuum. 4 was used
in the subsequent hydrolysis without any further purification,
crude yield 80%.1

Here is the original forensics work up from the twodogs proceedures. Obviously it varies a little from the OP here as the method here makes sodium perborate in situ. I'm just trying to make sense of the ratios.
 

G.Patton

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Are you sure your a chemist? I don't mean to be rude but DCM is not an NPS in the traditional sense.
It sounds rude. Do you know forum rules? You are right, i was wrong about DCM, I thought it vice versa. And yes, I am chemist actually but don't want to answer you any more.

solvent and relative polarity:
hexane 0.009
chloroform 0.259
methylene chloride 0.309
acetic acid 0.648
 

Fenster

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It sounds rude. Do you know forum rules? You are right, i was wrong about DCM, I thought it vice versa. And yes, I am chemist actually but don't want to answer you any more.

solvent and relative polarity:
hexane 0.009
chloroform 0.259
methylene chloride 0.309
acetic acid 0.648
Ok, thanks.

Do we have a definitive answer though. Has this been tested and developed in house or is this method scraped from somewhere else?
 
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@Fenster actually i dont even understand your problem but it seems you dont even understand what will be "generated in situ"

what you need is peracetic acid and this can be generated in situ by adding sodiumperborate to acetic acid,

second way is by mixing h2o2 with acetic acid and a tiny little bit h2so4. this is best to let it sit for a few days.

this method works, i tried it myself. Dont ask me for my exact h2o2:GAA ratio because mine again was a bit different and i only used 35%h2o2

only because of varied quantities of whatever it does not mean that one way does not work but the other does.
if you understand what's happening, then you'll be able to do small adjustments but if you dont understand whats happening then better do not claim a method to be bullshit
 

Fenster

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Sodium Perborate is insanely cheap and easy to acquire so why use Peroxide at all?
 

Felix34-73

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2) The solvent is evaporated under vacuum. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) 800 g how many degrees and how many mm hg pressure here
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3) evaporated under vacuum. 1-Phenyl-2-propanone yield 650 g. how many degrees is this how many mm hg pressure
 

Fenster

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2) The solvent is evaporated under vacuum. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) 800 g how many degrees and how many mm hg pressure here
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3) evaporated under vacuum. 1-Phenyl-2-propanone yield 650 g. how many degrees is this how many mm hg pressure

2) There isn't much information about this compound. I got a yellow oil after the DCM stopped coming over.

3) there is a lot of tar as a side product. I couldn't concentrate the vapour enough to get enough vapour to distill even under vacuum. I'm going to run this through on a larger scale then I did (I ran 100g of Benzaldehyde through) if I still have trouble getting the P2P to come over I'm going to steam distill everything including the DCM, the p2p should come over with the h20 and dissolve straight into the DCM where it can be separated. Like a an essential oil Distillation.
 

Felix34-73

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For the pH neutral process, I will use sodium carbonate + how many Gr, I will make the pH in the separating funnel neutral, I can make the scarbonate and water mixture directly in the solution and bring it to pH 7 level.
 
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