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Benzaldehyde and MEK - TwoDogs Method

Newbee

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can anybody provide me receipt to it
 

lalalander

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When 10 grams of Benzaldehyde + 10 grams of MEK and 7 grams of 30.5% aqueous HCl are mixed for 24 hours at room temperature, I obtain an organic layer.

The reaction should be carried out in an inert reactor, and the mouth of the reactor should be sealed with an inert stopper (such as LDPE, Teflon, glass, etc.).

I wash the organic layer with NaHCO3 solution until it is neutral and put it directly into the freezer. No heating. I filter it using a vacuum cleaner motor. This separates the remaining residual Benzaldehyde and MEK. White crystals remains behind.

When I pour -18 degree methanol on it, I obtain completely snow-white crystals. In my last test, I used 50 grams of Benzaldehyde + 50 grams of MEK and 35 grams of 30.5% aqueous HCl. I obtained 46 grams of snow-white crystals.

Methanol must be cooled in the freezer. Otherwise a lot of crystal will dissolve in the washing step.

I also think you can use ice water when washing, but I haven't tried it yet.
 
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lalalander

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My "P2P" smells very much like "burnt" benzaldehyde. After a while it starts to resemble apple flavor. There is also a very light honey note. But it smells predominantly like burnt benzaldehyde. And it takes hours to steam distill any usable amount. If I hydrolyze the ester separately with NaOH solution, a very dominant methyl acetate smell is emitted from the mixture.
 

LabPsycho

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I just wash the ester solution 2 times with water, and the acetic acid smell is gone.
 

AKINCI

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How does it become P2P?
 

LabPsycho

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I'm little bit confused. Are you asking me? If you are, what "it"? And if you are talking about acetoxyphenylpropene, don't ask from me because like you see, people get also confused. Confused from the smell of phenylpropanone. :)
 

LabPsycho

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What I mean, is not to be an ass. I have just seen very weird questions lately. Like how do you make a compound from a to b to c, when the whole procedure is known in here, or at least written the whole synthesis procedure in here! All I can say for those kind of ... weirdness is that I don't know shit about nothing.
 
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