Phenylacetone (P2P) synthesis from benzaldehyde with butanone

MadHatter

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Even in a scaled-down version.
 

WillD

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Excess acts as a solvent for the reaction. In terms of accessibility, try to use food vinegar concentrate. But with an excess of water, you need to think about an additional solvent.
 
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MadHatter

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No proble
No problem finding 60% concentration in large amounts. Would that suffice, or would I need to dehydrate it first?
 

WillD

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Yes, rather an excess of water will make unstable acid, unless it works in situ, but it is unlikely to be in time. You can try distillation or extraction.
 
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WillD

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There is also an alternative route. Use hydrogen peroxide and soda ash (sodium carbonate, Na2CO3) for creating sodium percarbonate, a strong oxidizing agent, as is peracetic acid. The reaction will be different, but in the end with the same result.

Edit: rather, baking soda (NaHCO3) can be used to form an epoxide followed by hydrolysis (analog Weitz-Scheffer epoxidation reaction)
 
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ASheSChem

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so, you think we can do 2-Acetoxy-1-phenyl-1-propene with sodium percarbonate ? any idea for the recipe ?
 

Mr.Blanks00

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halo, salam kenal, saya peserta baru di sini dari Indonesia, saya ingin bertanya kepada semua ahli kimia, saya membuat p2p dari asam penilasetat dan timbal dan asam glasial dalam botol stainless steel, saya mendapatkan hampir 100% minyak kuning dan merah dan air, saya ingin bertanya apakah minyak kuning itu penilaseton, dan bagaimana cara mencucinya dari kontaminan lain, terima kasih kepada semua ahli kimia yang mau menjawab pertanyaan saya.
 

Mr.Blanks00

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hello, nice to meet you, I'm a new participant here from Indonesia, I want to ask all chemists, I made p2p from penylacetic acid and lead and glacial acid in a stainless steel bottle, I got almost 100% yellow and red oil and water, I want to ask if the yellow oil is penylacetone, and how to wash it from other contaminants, thank you to all chemists who want to answer my question.
 

cokemuffin

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What would you suggest using if chloroform is not available?
 

Jamroz

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I will prepare hcl gas from sulfuric acid and hydrochloric acid, can anyone tell me what amount I need hcl and h2so4? when i know i have added enough gas?
 

waltjr5858

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I can tell you in this same reaction Scaled down They used 200 g of benzaldehyde to 300 G of MEK. I'm not sure which one of those that you base your gas addition on but they added until the mixture was 40 G heavier. So again I am not sure whether you can interpolate that with the benzaldehyde or the MEK depending on what scale you're using but I do know the weight came from a good resource. With this reaction on this site they use a 50/50 benzaldehyde MEK. I can try to look around and I'll let you know if I find something concrete
 

UWe9o12jkied91d

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I would say DCM, but I might be wrong
You also easily make chloroform by reacting cold 0* C bleach with acetone in stoechiometric amounts with a small 10% ish molar excess of bleach.Nilered has a video.
 

waltjr5858

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Imagine how many bottles of bleach you would have to use to make the chloroform needed for any sizable reaction. I do know that toulene works just fine and since that is easily purchasable that's what I would use
 

cokemuffin

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I saw the video, but i'm mainly interested in large scale manufacture, getting 6l chloroform that way is not really cheap and efficient. I'll probably try to further chlorinate DCM to chloroform.
 

TotalSynthesis

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Did anybody try this with caro's acid instead of GAA?
It should get a much better yield, at least i guess i read that somewhere but cant find any paper.

In the Peracetic way, GAA will also be the solvent but when using Caro's acid, i guess our precursor wont be soluble in the H2SO4 H2O2 mixture. Any idea which solvent could be used with Caro's ?
 

MadHatter

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I would be a bit weary mixing a ketone with caros acid ...
 

ASheSChem

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we need to obtain a certain PH or something ?
if we doing the method in a lower quantities, it's 1.5h too?
 

Mo0odi

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Methyl ethyl ketone is there an alternative

💝thank you all
 
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Fenster

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Im going to try this synth with dichloro-methane (DCM). I don't see this being an issue only that it will be heavier then water. Any reason to not use readily available DCM and synth Chloroform?
 
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