1-Phenyl-2-propanone (P2P) synthesis from Diethyl(phenylacetyl)malonate

ryan

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anyone can help
After completing a five-hour reflux, I transferred the mixture to an ice bath and intended to make it alkaline pH(12)

Initially, everything was going well, but I made a mistake and raised the pH to 14, causing the mixture to clot.

Can the mixture still be used?"
 
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ryan

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(picture 1)

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(Picture 2)

Sir, I need your help. I performed reflux for 7 hours at 55 degrees Celsius, with boiling chips already in the flask. After refluxing, I placed the mixture in an ice bath and added approximately 260 ml of 20% NaOH solution to make the mixture alkaline (pH 13). However, once the mixture became alkaline, it turned into irregular clumps (Picture 1). After that, I added 50 ml of diethyl ether to the mixture, and the clumps became uniform and floated on top of the mixture, as shown in (Picture 2.)

What happened? Did I make a mistake
 
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hacke8

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You use acid BMK, right? The reflux temperature is best at 70-75. 4 hours, cooling after completing the reaction, there is no need to adjust the PH to 13, PH7 is enough, use DCM to extract RM, P2P purification to check other threads.
 

ZMI_AA0B

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Idol, which top mixer is suitable? Because I collected 800 milliliters of diethyl malonate and wanted to synthesize phenylacetone
 

hacke8

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The greater the power, the better. The stirring paddle should be made of PTFE. The taste of this product 20320-59-6 is really unacceptable to me. It will linger on you.
 

ZMI_AA0B

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Teacher, may I ask how diethyl malonate is converted into diethyl phenylacetyl malonate
 

ZMI_AA0B

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How does diethyl malonate turn into diethyl phenylacetyl malonate
 

ZMI_AA0B

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It turns out that diethyl phenylacetate and diethyl malonate are different
 

ZMI_AA0B

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May I ask what to do if there is a shortage of phenylacetyl in diethyl malonate
 

VectorLaboratories

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I am about to carry out this synthesis but I am worried I might encounter some problems that have been discussed on this thread.

A user reported an intermediary product with a low boiling point which led to the user losing product in the condensation.

@G.Patton suggested that more pressure needs to be created in the system.

How can we do this when using one of the reactors shown in the video?
 

B APPLE

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請問你要加40毫升還是240毫升蒸餾水?
 

B APPLE

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爲什麼我們不能用乙醚分層?
 

B APPLE

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Is it normal for the solution to become cloudy after being extracted three times with ether and washed with 200ml of water
 

B APPLE

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Excuse me, teacher! How to restore the dark red color of phenylacetic acid and phenylacetone that I synthesized
 

G.Patton

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What do u mean "restore red color"???
 

B APPLE

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Thank you, teacher! I found the reason. Thank you
 

B APPLE

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After using the method taught by the teacher, I finally succeeded with phenylacetone
 

B APPLE

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Can you please advise on a relatively simple method for synthesizing methamphetamine from phenylacetone? Thank you!
 
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