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

[G.Patton]

Diethyl ether (Et2O) ~150 mL;

ZeteticHi, it can be replaced by Petroleum ether

Glacial acetic acid (AcOH) 60 mL;

you can use acetic acid 70% but you have to recount volume of water

Concentrated sulfuric acid (H2SO4) 7.5 mL;

you can't replace it

 

[Ra226]

Hi, it can be replaced by Petroleum ether

you can use acetic acid 70% but you have to recount volume of water

you can't replace it

G.PattonH₂SO₄ can also theoretically be substituted.On the premise of using anhydrous acetic acid, you add 40ml of water to 7.5ml of sulfuric acid, so if you don't add water at all, you can use sulfuric acid with a concentration of 34% to 35%. Converted by weight, this only requires the use of slightly concentrated battery electrolyte

 

[cokemuffin]

Are there changes in the procedure if you use ethyl 3-oxo-4-phenylbutanoate (CAS 718-08-1)?

 

[G.Patton]

Are there changes in the procedure if you use ethyl 3-oxo-4-phenylbutanoate (CAS 718-08-1)?

cokemuffinFor 3-oxo-4-phenylbutyrate reaction is different.

 

[LordCrackingtonson]

For 3-oxo-4-phenylbutyrate reaction is different.

G.PattonHello Mr Patton.. have a question regarding the ethyl ester of 3-oxo-4-phenylbutyrate.

Ethyl 3-oxo-4-phenylbutyrate CAS no. 718-08-1

Can you help with conversion instructions for this to P2P?

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/help-with-conversion-of-bmk-powder-718-08-1-to-p2p.6017/

​

 

[Bartholomeus]

Why is here needed to use 2 acids? Glacial acetic acid + sulfuric acid?
And should the b powder be added to hot GAA+h2so4+water mix so it will dissolve easier?
And at least which water proportion is correct 240ml or 40ml per 55g powder?

 

[Never to sleep]

Anyone willing to share a tested trustworthy source for the Diethyl(phenylacetyl)malonate?

 

[G.Patton]

Anyone willing to share a tested trustworthy source for the Diethyl(phenylacetyl)malonate?

Never to sleepYou can use BB Escrow to protect your money and order here. It can be found via Search in BB Listing.

Diethyl(phenylacetyl)malonate cas 20320-59-6 in stock

Product Name Diethyl 2-(2-phenylacetyl)propanedioate Synonyms Diethyl(phenylacetyl)malonate;Propanedioic acid, 2-(2-phenylacetyl)-, 1,3-diethyl ester;diethyl 2-(2-phenylacetyl)propanedioate;diethyl 2-(2-phenylacetyl)propanedioate wickr...

bbgate.com

 

[kwisspeed de Kelog's]

when you say add a solution of glacial acetic acid of 60ml, should I put 60ml of pure or diluted acid? knowing that I use 99% glacial acetic acid. I apologize for my newbie questions and thank you in advance.

 

[G.Patton]

when you say add a solution of glacial acetic acid of 60ml, should I put 60ml of pure or diluted acid? knowing that I use 99% glacial acetic acid. I apologize for my newbie questions and thank you in advance.

kwisspeed de Kelog'sno, you shouldn't dilute it.

 

[kwisspeed de Kelog's]

Hello everyone, please could someone explain to me more precisely the step where we must add the three portions of ether. I am sincerely sorry, I am a beginner and do not understand this step well.
I thank you for all your precious help.
I show you a picture of the result I get, before adding the portions of ether.

 

[G.Patton]

Hello everyone, please could someone explain to me more precisely the step where we must add the three portions of ether. I am sincerely sorry, I am a beginner and do not understand this step well.
I thank you for all your precious help.
I show you a picture of the result I get, before adding the portions of ether.

kwisspeed de Kelog'sHello, please, learn Laboratory FAQ section and this topic: Extraction

 

[Lwx601109]

hello @G.Patton and anybody answer some doubts? i have som doubts about reaction temperature,
1 . the mixture refluxed in 500 mL round bottom flask with reflux condenser for four or five hours until the decarboxylation was complete ，What is the temperature?
2. and the solvent distilled off, What is the temperature?
3. The residue containing the ketone (2) was distilled in vacuo to give 1-Phenyl-2-Propanone (2) in 71 % What is the temperature?

thanks very much， from a newbie

 

[G.Patton]

hello @G.Patton and anybody answer some doubts? i have som doubts about reaction temperature,
1 . the mixture refluxed in 500 mL round bottom flask with reflux condenser for four or five hours until the decarboxylation was complete ，What is the temperature?
2. and the solvent distilled off, What is the temperature?
3. The residue containing the ketone (2) was distilled in vacuo to give 1-Phenyl-2-Propanone (2) in 71 % What is the temperature?

thanks very much， from a newbie

Lwx601109

What is the temperature?

Reflux = boiling = boiling temperature.

and the solvent distilled off, What is the temperature?

solvent boiling point temperature

What is the temperature?

Depends on your applied vacuum.

Please, read Laboratory FAQ section and everything have to be more clearly after. There are topics about heating, boiling point, distillation.

 

[Lwx601109]

Reflux = boiling = boiling temperature.

solvent boiling point temperature

Depends on your applied vacuum.

Please, read Laboratory FAQ section and everything have to be more clearly after. There are topics about heating, boiling point, distillation.

G.PattonOk, very helpful for your advice, thank you very much @G.Patton

 

[w2x3f5]

This reaction also goes with phosphoric acid

 

[LordCrackingtonson]

This reaction also goes with phosphoric acid

w2x3f5The original synthesis on page 1 calls for 7.5ml concentrated sulphuric acid.

If you substitute 85% phosphoric acid instead, how much would be required?

 

[LordCrackingtonson]

I did several times, mixed the oil 1 to 1 with phosphoric acid, heated it until the gas evolution stopped. Unfortunately, I did only a few hydrolysis and did not record.

w2x3f5Did you use glacial acetic acid and phosphoric acid together.. or just equal amounts phenylacetylemalonate and phosphoric acid?

 

[w2x3f5]

Did you use glacial acetic acid and phosphoric acid together.. or just equal amounts phenylacetylemalonate and phosphoric acid?

LordCrackingtonsonH3PO4 only

 

[huhahuha]

Thank you for the video！
but how to preparation
Diethyl(phenylacetyl) malonate?
I can't buy this thing here...
Do you have any good method?

 

[41Dxflatline]

Some bees buzzed that diethyl(phenylacetyl)malonate could be used directly in a Leuckart reduction without first being converted to P2P

 

[w2x3f5]

Some bees buzzed that diethyl(phenylacetyl)malonate could be used directly in a Leuckart reduction without first being converted to P2P

41Dxflatlineduring the hydrolysis of malonate, impurities in the ketone, the color of the ketone is more dirty than with glycidate

 

[41Dxflatline]

during the hydrolysis of malonate, impurities in the ketone, the color of the ketone is more dirty than with glycidate

w2x3f5Never used it, they mentioned it in passing on the vespiary as possible but none of them seemed to have actually tried it

 

[w2x3f5]

Never used it, they mentioned it in passing on the vespiary as possible but none of them seemed to have actually tried it

41DxflatlineI use with H3PO4 hydrolysis, but one or two times