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

[ryan]

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?"

 

[ryan]

Hello,okay thank you sir

 

[ryan]

(picture 1)

(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

 

[hacke8]

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]

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

 

[hacke8]

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]

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

 

[ZMI_AA0B]

How does diethyl malonate turn into diethyl phenylacetyl malonate

 

[ZMI_AA0B]

It turns out that diethyl phenylacetate and diethyl malonate are different

 

[ZMI_AA0B]

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

 

[VectorLaboratories]

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?