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

OrgUnikum

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Guys, do not fall for the cult of the holy reflux. Refluxing has no worth in itself except for the illusion of something happening which it creates.

With H2SO4 and Oxalic acid (best) but Phosphoric Acid and about any organic acid like Acetic or Formic or Citric work one gets next to quantitative yields if one heats up the mixture slowly over two hours to NOT MORE then 95 °C, holds it there for 30 minutes and then let it cool down. Add a small amount of solvent other then DCM (Toluene, Xylene, Ether) as organic acid may fall out and so collecting from top is advised. Petrol Ether 40/60 can be used and not much is needed but you get THREE layers in the end: Top layer is Pet-Ether with P2P dissolved. Middle layer is P2P with Pet-Ether dissolved*. And below is the acid mix (which can be re-used btw. without problems).

*Sounds funny but thats how it is: Both, Pet-Ether and P2P dissolve some of the other one but thex are not freely miscible. And so you get the three layers which drove me next to nuts already a long time ago. Until I figured this out.......

200 g Oxalic Acid Dihydrate
300 ml Water
100 ml H2SO4 37% (battery acid)
not all Oxalic Acid will dissolve - no problem
With this one can process a minimum 200 ml 20230 red oil
Really strong stirring all the time is needed.
The water/acid mix can be re-used.
Not over 95 °C gives light yellow P2P directly without steam or other distillation.
When you use a sep-funnel you best separate as long its still hot and the oxalic does not drop out.Or you put it in a beaker in the freezer with the bottom of the beaker touching the cold so it starts to crystallize from there. If you do this you need no solvent at all, the acid and watere crystallizing from the bottom will drive the P2P to the top and you can just pour it out after two or three hours and NO P2P will be left back.

I did a lot of work on this one, lol
 
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ZMI_AA0B

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Teacher, can phenylacetone be synthesized using only oxalic acid, water battery acid, and these three materials
 

w2x3f5

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indicate the yield of the substance p2p please.
do you have red oil? strangely, I had yellow oil under the same number.
 
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OrgUnikum

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How does it smell? But anyways it should be light yellow to golden at most (lighter color is better), it is really quite easy, red oil + water + oxalic acid + 38% H2SO4, heat to a max. of 95°C hold at this temp for some time and let cool down. STRONG STIRRING is most important! Until it is finished and let cool down of course.
Theoretical max. yield is about 45g P2P from 100g 20320-59-6, my yield was never less then ~40g of high quality P2P from 100g starting material after I had figured the method out, which is btw. very close to the method the inventor of the synthesis used and published in the article he wrote about it.

 

OrgUnikum

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Look there are two possibilities:
First: You do not have 20230-59-6 but something else
Second: You thnk you did what I wrote but on a closer look you did not due to some misunderstanding/language issues or whatever.

I would guess number two is it, after my experience it will be .
 

ZMI_AA0B

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Teacher, may I ask which type of red oil it is
 

ZMI_AA0B

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Excuse me, is it Türkiye red oil?
 

ZMI_AA0B

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What kind of solvent is diethyl acetate (phenylacetyl) malonate
 

G.Patton

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Hello, it is not a solvent. It is the precursor for P2P. Diethyl(phenylacetyl)malonate cas 20320-59-6.
 
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ZMI_AA0B

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Teacher, is it acetophenone?
 

G.Patton

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

ZMI_AA0B

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

ZMI_AA0B

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Teacher, does ephedrine need to be neutralized before synthesizing amphetamine and ephedrine? I didn't know before that a lot of ephedrine was wasted, so I wanted to finish the remaining materials first
 

ZMI_AA0B

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Teacher, do you know N-phenylethyl ketone
 

hacke8

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Hi, my friend, judging from the question you sent. Your chemical foundation is zero. I recommend you take a look at the introduction to chemistry first, heating, stirring, filtration, extraction, anti-extraction, and some simple chemical equipment, flasks, beakers, liquid separation funnels, and some other basic chemical supplies. In this way, you can more easily understand some threads published by BB Forum.
 

ZMI_AA0B

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Thank you, teacher. I will study hard
 

ZMI_AA0B

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How to synthesize diethyl phenylacetylmalonate
 

ZMI_AA0B

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Teacher, how does malonic acid synthesize diethyl malonate?
 

ryan

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IlkqYCsUOz


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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G.Patton

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Hello, 12 and 14 pH difference can't cause this problem. Probably, there is unreacted precursor or its admixture/impurities. You can filter it and steam distill for a following usage.
 
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