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Synthesis of P2P from benzaldehyde with MEK (1kg scale)

William Dampier

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Step 1. 3-methyl-4-phenyl-3-buten-2-one.
1. Mixed 1000 g benzaldehyde and 1000 ml MEK, stirring and chilled at 0 *C.
2. HCl gas was bubbled slowly through a mixture 1.5 hours.
3. The solution was stirred for 1.5 hours at room temperature.
4. Water was added, and the solution extracted with chloroform, then washed with sodium bicarbonate solution and dried (Na2SO4).
5. Solvent was removed under high vacuum and 3-methyl-4-phenyl-3-buten-2-one was distilled under vacuum (bp.76-78 *C). Yield: 1000 g.

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Step 2. 2-Acetoxy-1-phenyl-1-propene.
1. Product from Step 1, 10000 ml glacial acetic acid and 1300 g 50% H2O2 was stirring and heated at 55 *C for 23 hours.
2. After this time water added 10000 ml water.
3. Extracted with 5000 ml chloroform.
4. Solvent removed under vaccum to yield 800 g of 2-Acetoxy-1-phenyl-1-propene.


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Step 3. 1-phenyl-2-propanone.
1. Product for Step 2 and 600 g sodium hydroxide in 2500 ml water was stirred at 50 °C 12 hours.
2. Solution extracted with 1000 ml chloroform, dried (Na2SO4) and the solvent removed under vacuum. Yield: 650 g.
 
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cyb3r0

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Thank you for the explanation. Please mention the required materials that you knew
benzaldehyde and Methyl Ethyl Ketone ( MEK )
Is this all that is required?
Thank you
 

DocX

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Thank you so much for the easy and detailed synth description!
How about the hydrogen peroxide, could that be substituted? It's a really controlled chemical nowadays, and a bitch to synthesize yourself. Its mainly there as a catalyst in the reaction between the glacial acetic acid and the 3-methyl-4-phenyl-3-buten-2-one, right? What could be a good substitute?
 
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Jack

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Its mainly there as a catalyst in the reaction between the glacial acetic acid and the 3-methyl-4-phenyl-3-buten-2-one, right? What could be a good substitute?
It is not a catalyst it is an oxidant please read the link provided, search up baeyer villiger oxidation.
 

DocX

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It is not a catalyst it is an oxidant please read the link provided, search up baeyer villiger oxidation.
Ok, good, an oxidant. And I see the reaction in the link. Thank you! In it they use sodium perborate for the BV- oxidation. That might be more accessible. I guess piranha solution could be used also? What other candidates are there?
 
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DocX

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After reading up a bit: how about sodium percarbonate? Would that suffice? Because if it would, this synthesis would become much more OTC. And definately worth the time to calculate the molar ratio.
 

William Dampier

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Approximately 3kg percarbonate for this reaction+water. Find a concentrated peroxide is best choice.
 

DocX

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That's perfectly doable. Of course it's second best, but hydrogen peroxide in concentrations above 3% is a strictly controlled substance nowadays in most of EU.
One thought though: wont the carbonate ion react really vividly with the acetic acid? And maybe neutralize it?
 

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Is it necessarliy to make it under vacum destilation or normal pressure destilation will be enought ? Could you expand first step in the reaction hcl gas bubbled in mixture
 

n00by Blitz

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1. Product from Step 1, 10000 ml glacial acetic acid and 1300 g 50% H2O2 was stirring and heated at 55 *C for 23 hours.
Just to confirm. It is: 10 liters of glacial acetic acid. Am I correct?
 
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a_king

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is it possible to replace chloroform?
 

DocX

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is it possible to replace chloroform?
Why would you want to replace chloroform? It's easy to synthesize yourself with acetone and bleach. Check youtube.
But if you really need to for some reason, dichloromethane and chloroform are usually interchangeable.
 

DocX

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BTW, why such ENORMOUS quantities of GAA and H2O2? Is it possible to use less? What are their roles in this reaction?
 
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DocX

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I guess what I'm really wondering about is the stochiometry of this reaction. In other write-ups of the bayer-williger I can't seem to find this enormous amounts of GAA. Can somebody help me with the rationale? I'm really close to trying this one out, but the amount of GAA is problematic.
 
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