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

[btcboss2022]

I made this process with success!
We are just trying to fix a small problem with salt precipitate in the alkalination phase.
I'm very grateful to G.Patton for all his help great expert thanks again.

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[hello999]

Perform CAS 20320-59-6 official procedure After 4 hours of reaction at 80°C, stop heating, then adjust the alkali pH with sodium hydroxide, until 7, it can't go up, stratification appears, the oil layer is on top, and then ether extraction is added, and the stratification begins, and the ether layer is extracted, and the upper layer starts, and the distillation at atmospheric pressure at 220° keeps going up, and the temperature keeps it at 110°, and a lot of liquid is distilled, and I think it's ether, and then it starts to appear, and this phenomenon in the flask I thought it would be 216° distillation to produce P2P, but there is no problem How can I remedy it

 

[hacke8]

Hello, have you solved the problem that you can't get 12 on PH? I also encountered the same problem. Please help me. Thank you.

 

[qwe111]

Sir: How many hours does this reaction process take? Within what range should the temperature be controlled? What is the target pH value for adding sodium hydroxide?

 

[G.Patton]

Hello, what reaction exactly do u mean? Should I guess?

 

[qwe111]

Sir, I failed again!
I want to ask more carefully. How many times should 115 grams of sodium hydroxide solution be added? How long should the interval be?
What should be the pH value after adding alkaline?

 

[qwe111]

I obtained a solid, a yellow salt, by adding twice as much sodium hydroxide solution. I don't know if this is right?

 

[G.Patton]

Have you checked your precursor?

There is no difference how many time. It's important to avoid the reaction overheating.
Have you added 115g NaOH to 800g of Diethyl(phenylacetyl)malonate? You add equimolar amount of NaOH to make hydrolysis with following salt formation.

 

[qwe111]

Sir, I have newly ordered 20320-59-6.
I added 115g Naoh to 800g20320-59-6 and could not get a solid.
I did 2 complete experiments today.
The temperature of the sodium hydroxide solution is normal when slowly added, but a solid cannot be obtained. I tried adding more solution and the temperature stayed stable. The liquid suddenly solidified when about twice as much sodium hydroxide solution was added. And the temperature rises to 80°. Get yellow salt.
After drying, add one liter of water and heat to 60°. The mixture will foam a lot.
Return to normal after adding hydrochloric acid.
The oil obtained after 1 hour is on the bottom layer. No crystallization after placing it in the refrigerator.
Sir, please help me. what should I do?
Thank you very much! !

 

[G.Patton]

Check boiling point of this oil. If it is not okay, steam distill it. That's all. =)

 

[G.Patton]

Does your solid product after NaOH addition has any smell?

 

[qwe111]

Smells like penicillin. You will feel chest tightness without wearing a respirator. This smell will not evaporate for many days. Always present indoors, on clothes, on the body.

 

[qwe111]

Good morning, dear Mr. G. Patton:
I was just thinking and suddenly got some inspiration.

I tested the pH value of a mixture of sodium hydroxide solution added during an experiment a few days ago. I probably remember it as neutral. This shouldn't be right. So what should be the correct pH value?

Dissolve the salt of 20320-59-6 in one liter of water, turn on stirring and heat to 60°. After all is dissolved, add hydrochloric acid. Reaction takes 1 hour. Should I turn off the heater after adding hydrochloric acid?

Looking forward to your reply.
Thank you very much!
Good luck with your work!

 

[G.Patton]

It should be alkaline ~12.
Yes, it has to be.

 

[qwe111]

my God. No wonder it fails so many times. I wasted about 3KG20320-59-6. and several liters of hydrochloric acid. Hydrochloric acid is hard to get in my country =.=! I spent a lot of money.

The pH value of the solid obtained is wrong.
After adding the hydrochloric acid, I continued to heat to maintain the temperature at 60-65°.
I'm so stupid.

Thank you for your patient answer sir!

 

[G.Patton]

it's correct
Yes, you should.
This is assumed that the mixture is heated during hydrolysis

I told about pH after NaOH sln addition

I guess your problem is with your 20320-59-6. You don't check it and spend reagents for nothing.

 

[qwe111]

sorry sir
I'm an idiot who doesn't know anything about chemistry.
My English is not good either. A translator is required. It may be a translator problem and I can't understand your answer.

Is the mixture self-heating?

My understanding is that after adding hydrochloric acid, the temperature should be kept at 60-65° for an hour. If the temperature is too low, you need to turn on the heater. If the temperature is too high, it needs cooling, right?

I found two new suppliers yesterday and ordered 2 copies of 20320-59-6. I will continue to experiment tomorrow.

Thank you.

 

[G.Patton]

Yes, a little. Nevertheless, you need to apply external heating.
I'm writing 3rd time, yes, it is correct. You can heat it 60-90*C. This range is okay.

 

[qwe111]

Dear Mr.
Add the sodium hydroxide solution and stir until the mixture becomes solid.
Correct Procedure How long does this need to be stirred? a couple of hours?

 

[qwe111]

gentlemen.
Another expert told me it needs to be stirred for 12 hours or more. I want to know is this correct?

 

[G.Patton]

Hello, correct. Do you think he try to mislead you? =)

 

[qwe111]

No sir.

I just trust you.

I think you are very knowledgeable! So I trust you more!

I made mistakes in my previous experiments. My mixing time is too short each time. I continued to add the sodium hydroxide solution when I saw that the mixture would not become solid. resulting in the addition of excess solution. and get the wrong stuff.

Now I'm so sad! ! !

 

[ZMI_AA0B]

Unable to understand the first type of material

 

[ZMI_AA0B]

What kind of solvent is diethyl acetate (phenylacetyl) malonate

 

[G.Patton]

Hello, it is not a solvent. It is the precursor for P2P. Diethyl(phenylacetyl)malonate cas 20320-59-6.

 

[G.Patton]

So, what interfere you to use it? I sent you name and cas.

 

[ZMI_AA0B]

Hello teacher, as I am an Australian, it is difficult to find the materials, but I should be able to find them all