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]

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.

photo-2022-05-04-14-24-05

Image photo-2022-05-04-14-24-05 hosted in ImgBB

ibb.co

photo-2022-05-04-14-24-09

Image photo-2022-05-04-14-24-09 hosted in ImgBB

ibb.co

photo-2022-05-06-12-53-27

Image photo-2022-05-06-12-53-27 hosted in ImgBB

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btcboss2022Perform 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

 

[btcboss2022]

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 View attachment 32686 View attachment 32687 View attachment 32688 View attachment 32689 View attachment 32690

hello999There is a detailed video of that process seems easy.

 

[hacke8]

There is a detailed video of that process seems easy.

btcboss2022Hello, have you solved the problem that you can't get 12 on PH? I also encountered the same problem. Please help me. Thank you.

 

[rothschild33]

Performed the 20320 -> PAA and Phenylacetone method,


1. An alkali aqueous solution 50 % is prepared in advance so that it has time to cool down. Sodium hydroxide 115 g (NaOH) is dissolved in water 115 g and cooled down to room temperature.
2. The cooled NaOH aqueous solution of is poured into a dropping funnel and this funnel is installed onto a reactor.
3. Diethyl(phenylacetyl)malonate 800 g is poured into the reactor. The reaction is carried out at room temperature but a forced cooling can be used during the hydrolysis.
4. A stirrer is turned on and NaOH aq solution adding is begun slowly. Reaction temperature has to be controlled (the mixture is self-heated). As the solution is added, reaction mixture (RM) color is changed and thickened until it is become completely thick and lumpy. The lumps is broken into a homogeneous mass.

After adding the NaOH, the mixture turns lighter and lighter over the course of minutes getting thicker. Then, at one point the mixture turns back into the color of 20320-59-6.

This was the mixture color after a few minutes of NaOH addition

As time progressed, it started reverting back to the original color:

Then afterwards it just remained in this state:

Anyone know what I can do to fix this, any trial and error / troubleshooting methods?
Also what should I research, what kind of reaction is this, so I could dig deeper into the optimal reaction condition?

 

[qwe111]

Performed the 20320 -> PAA and Phenylacetone method,


1. An alkali aqueous solution 50 % is prepared in advance so that it has time to cool down. Sodium hydroxide 115 g (NaOH) is dissolved in water 115 g and cooled down to room temperature.
2. The cooled NaOH aqueous solution of is poured into a dropping funnel and this funnel is installed onto a reactor.
3. Diethyl(phenylacetyl)malonate 800 g is poured into the reactor. The reaction is carried out at room temperature but a forced cooling can be used during the hydrolysis.
4. A stirrer is turned on and NaOH aq solution adding is begun slowly. Reaction temperature has to be controlled (the mixture is self-heated). As the solution is added, reaction mixture (RM) color is changed and thickened until it is become completely thick and lumpy. The lumps is broken into a homogeneous mass.

After adding the NaOH, the mixture turns lighter and lighter over the course of minutes getting thicker. Then, at one point the mixture turns back into the color of 20320-59-6.

This was the mixture color after a few minutes of NaOH addition
View attachment 17347


As time progressed, it started reverting back to the original color:

View attachment 17348


Then afterwards it just remained in this state:



View attachment 17349


Anyone know what I can do to fix this, any trial and error / troubleshooting methods?
Also what should I research, what kind of reaction is this, so I could dig deeper into the optimal reaction condition?

rothschild33Sir: Have you successfully obtained pure phenyl acetone? Are there any additional steps? Have the ratios of any solvent additions been changed?

 

[Junjun888]

Execution Synthesis of phenylacetic acid and phenylacetone (P2P) from phenylacetylmalonic acid sodium salt 10. While the mixture is still hot, drain and discard the water layer at the bottom. The layers can be separated using a separatory funnel. Collect the top layer. Why is my product not at the top but at the bottom?

 

[Junjun888]

实施由苯乙酰基丙二酸钠盐合成苯乙酸和苯丙酮(P2P) 10.趁混合物仍热时，排出并丢弃底部的水层。可以使用分液漏斗分离各层。收集顶层。为什么我的产品不在顶部而是在底部？

Junjun888

 

[Junjun888]

Execution Synthesis of phenylacetic acid and phenylacetone (P2P) from phenylacetylmalonic acid sodium salt 10. While the mixture is still hot, drain and discard the water layer at the bottom. The layers can be separated using a separatory funnel. Collect the top layer. Why is my product not at the top but at the bottom?

Junjun888

 

[Junjun888]

View attachment 30243

Junjun888And put it in the refrigerator. There is no crystallization like in the video.

 

[WillD]

And put it in the refrigerator. There is no crystallization like in the video.

Junjun888Write in DM, I will help you.

 

[Beginner from China]

I want to ask, is this suitable for novices? What I call a novice is someone who doesn’t understand it at all.I took a look and the publication date for this is recent. In other words, is this the latest method?

 

[cokemuffin]

I want to ask, is this suitable for novices? What I call a novice is someone who doesn’t understand it at all.I took a look and the publication date for this is recent. In other words, is this the latest method?

Beginner from ChinaActually not, you should probably learn basic chemistry before you attempt any synthesis. Could work without the knowledge, but in case something goes wrong you can mess up pretty bad

 

[Beginner from China]

Actually not, you should probably learn basic chemistry before you attempt any synthesis. Could work without the knowledge, but in case something goes wrong you can mess up pretty bad

cokemuffinThank you. I'm currently studying basic knowledge and English

 

[WillD]

I want to ask, is this suitable for novices? What I call a novice is someone who doesn’t understand it at all.I took a look and the publication date for this is recent. In other words, is this the latest method?

Beginner from ChinaVery simple synthesis if the quality of your raw materials is ok. You can write to experts in DM, we will help with this.

 

[Beginner from China]

Very simple synthesis if the quality of your raw materials is ok. You can write to experts in DM, we will help with this.

William D.Thank you. Speaking of which. I have exactly one question. I searched for the required ingredients. But the prices vary greatly. My question is under normal circumstances, what grade of raw materials do we need?

 

[G.Patton]

Thank you. Speaking of which. I have exactly one question. I searched for the required ingredients. But the prices vary greatly. My question is under normal circumstances, what grade of raw materials do we need?

Beginner from ChinaMost of reagent should be Reagent grade. The purer reagent, the less side products and impurities in a final product.

 

[Beginner from China]

Most of reagent should be Reagent grade. The purer reagent, the less side products and impurities in a final product.

G.Pattonthanks

 

[qwe111]

Phenylacetyl-malonic Acid Sodium Salt From Diethyl(phenylacetyl)malonate

1. An alkali aqueous solution 50 % is prepared in advance so that it has time to cool down. Sodium hydroxide 115 g (NaOH) is dissolved in water 115 g and cooled down to room temperature.
2. The cooled NaOH aqueous solution of is poured into a dropping funnel and this funnel is installed onto a reactor.
3. Diethyl(phenylacetyl)malonate 800 g is poured into the reactor. The reaction is carried out at room temperature but a forced cooling can be used during the hydrolysis.
4. A stirrer is turned on and NaOH aq solution adding is begun slowly. Reaction temperature has to be controlled (the mixture is self-heated). As the solution is added, reaction mixture (RM) color is changed and thickened until it is become completely thick and lumpy. The lumps is broken into a homogeneous mass.
5. RM is moved from the reactor to a vacuum filtration system funnel and filtered. Phenylacetyl-malonic acid sodium salt is obtained.​

G.PattonSir: 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]

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?

qwe111

How many hours does this reaction process take?

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

 

[qwe111]

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

G.Patton1. An alkali aqueous solution 50 % is prepared in advance so that it has time to cool down. Sodium hydroxide 115 g (NaOH) is dissolved in water 115 g and cooled down to room temperature.
2. The cooled NaOH aqueous solution of is poured into a dropping funnel and this funnel is installed onto a reactor.
3. Diethyl(phenylacetyl)malonate 800 g is poured into the reactor. The reaction is carried out at room temperature but a forced cooling can be used during the hydrolysis.
4. A stirrer is turned on and NaOH aq solution adding is begun slowly. Reaction temperature has to be controlled (the mixture is self-heated). As the solution is added, reaction mixture (RM) color is changed and thickened until it is become completely thick and lumpy. The lumps is broken into a homogeneous mass.
5. RM is moved from the reactor to a vacuum filtration system funnel and filtered. Phenylacetyl-malonic acid sodium salt is obtained.

sorry sir.
thank you for your reply.
my question is
1: How many hours is the most reasonable time to add sodium hydroxide solution?
2: In what range should the temperature be controlled when adding sodium hydroxide solution?
3: What is the approximate dosage of 800g20320-59-6 hydrochloric acid to adjust the pH to less than 3?

Sorry again sir. Because the experiment failed, I felt complicated and sent some spam messages. I will not do it again. I wish you a happy mood!

 

[G.Patton]

1. An alkali aqueous solution 50 % is prepared in advance so that it has time to cool down. Sodium hydroxide 115 g (NaOH) is dissolved in water 115 g and cooled down to room temperature.
2. The cooled NaOH aqueous solution of is poured into a dropping funnel and this funnel is installed onto a reactor.
3. Diethyl(phenylacetyl)malonate 800 g is poured into the reactor. The reaction is carried out at room temperature but a forced cooling can be used during the hydrolysis.
4. A stirrer is turned on and NaOH aq solution adding is begun slowly. Reaction temperature has to be controlled (the mixture is self-heated). As the solution is added, reaction mixture (RM) color is changed and thickened until it is become completely thick and lumpy. The lumps is broken into a homogeneous mass.
5. RM is moved from the reactor to a vacuum filtration system funnel and filtered. Phenylacetyl-malonic acid sodium salt is obtained.

sorry sir.
thank you for your reply.
my question is
1: How many hours is the most reasonable time to add sodium hydroxide solution?
2: In what range should the temperature be controlled when adding sodium hydroxide solution?
3: What is the approximate dosage of 800g20320-59-6 hydrochloric acid to adjust the pH to less than 3?

Sorry again sir. Because the experiment failed, I felt complicated and sent some spam messages. I will not do it again. I wish you a happy mood!

qwe111

Reaction temperature has to be controlled (the mixture is self-heated)

Depends on your reaction size. Main Idea is that you have to add it as fast as temperature can be controlled.

2: In what range should the temperature be controlled when adding sodium hydroxide solution?

50-60*C is max

3: What is the approximate dosage of 800g20320-59-6 hydrochloric acid to adjust the pH to less than 3?

About 105g need to make it neutral and a little more to make it pH 3. You can play by ear with pH indicator paper during reaction.

Because the experiment failed

Check your reagents before synthesis. Your cas 20320-59-6 may be are not so well.

 

[qwe111]

Depends on your reaction size. Main Idea is that you have to add it as fast as temperature can be controlled.

50-60*C is max

About 105g need to make it neutral and a little more to make it pH 3. You can play by ear with pH indicator paper during reaction.


Check your reagents before synthesis. Your cas 20320-59-6 may be are not so well.

G.PattonOkay, thanks again sir.
I'll order a new copy of the materials and run the experiment again.

 

[G.Patton]

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

qwe111Hello, correct. Do you think he try to mislead you? =)

 

[qwe111]

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

G.PattonNo 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! ! !