Phenylacetone (P2P) synthesis via BMK ethyl glycidate

[chem19]

@G.Patton
can you pls clarify that in step 14 "(14. After a while, distilled water 500 ml is added and the mixture is heated a little (no more than 60°C).".

My question is how long it should be heated. (Time duration) or any sign.
Thanks in advance.

 

[jotoy]

@G.Patton
can you pls clarify that in step 14 "(14. After a while, distilled water 500 ml is added and the mixture is heated a little (no more than 60°C).".

My question is how long it should be heated. (Time duration) or any sign.
Thanks in advance.

chem19Hi and is it from this step that you stqrt if you have BMK 5449-12-7 powder or the new bmk powder in market now?

 

[chem19]

Hi and is it from this step that you stqrt if you have BMK 5449-12-7 powder or the new bmk powder in market now?

jotoyI started from Dimethylformamide, benzaldehyde exactly as in video.

 

[virus0815]

how much BMK glycidic acid (sodium salt) do i need for 1 gramm of P2P?

 

[61-50-7]

there is a little error : you said pmk instead of bmk in the first lines

 

[rampage]

View attachment 16107

This phenylacetone (P2P) synthesis approach is a simple way how to get phenylacetone from BMK ethyl glycidate and its synthesis from benzaldehyde. PMK ethyl glycidate can be hydrolyzed into P2P. This reaction isn't sensitive to water like BMK methyl glycidate synthesis. There is such advantage like a quite high yield conversion (82% from benzaldehyde to P2P). Moreover, the reaction doesn't take any elaborated equipment and can be easily scailed.​

Equipment and glassware:​

• Four necked round bottom reaction flask 3 L, equipped with reflux condenser, top stirrer and pressure equalized drip funnel 250 mL;​
• Funnel;​
• Retort stand and clamp for securing apparatus;​
• pH indicator paper;​
• Water/oil bath;​
• Retort stand and clamp for securing apparatus;​
• Laboratory grade thermometer (up to 10 - 100 °С);​
• Glass rod;​
• Silicone hoses;​
• Measuring cylinders for 100 mL and 1 L;​
• Laboratory scale (1-200 g is suitable);​
• Glass rod;​
• Beakers 3 L; 1 L x2; 500 ml x2;​
• Separatory funnel 2 L;​

Reagents:​

• Dimethylformamide 900 ml;​
• Benzaldehyde 300 ml;​
• Ethyl 2-chloropropionate 540 g;​
• Benzyltriethylammonium chloride (TEBAC) 32 g;​
• Potassium carbonate 780 g;​
• Sodium hydroxide (NaOH) 135 g;​
• Distilled water ~1.9 L;​
• Concentrated (37%) aqueous hydrochloric acid (HCl) ~250 mL;​

Download Video

Phenylacetone (P2P) Synthesis Via BMK Ethyl Glycidate

• Novator
• Jun 1, 2023
• 53
• 1-phenyl-2-propanone benzaldehyde bmk bmk ethyl glycidate bmk glycidic meth p2p synthesis

1) BMK ethyl glycidate synthesis from benzaldehyde.
2) BMK glycidic acid (sodium salt) synthesis...

​

BMK ethyl glycidate synthesis from benzaldehyde​

View attachment 16109 ​

1. Dimethylformamide 900 ml is poured into a 3 L four necked round bottom reaction flask, equipped with reflux condenser, top stirrer and drip funnel.​

2. Then, benzaldehyde 300 ml is added. A top stirrer is turned on.
3. Ethyl 2-chloropropionate 540 g is poured into the reactor. Benzyltriethylammonium chloride (TEBAC) catalyst 32 g is added. Next, potassium carbonate 780 g is added into the reaction mixture.
4. A heating of the water or oil bath is set at 40°C.
5. Reaction mixture is stirred for 48 h on the warm bath.
6. Sodium hydroxide (NaOH) 30% water solution 450 ml is prepared in advance.
7. After 48h, the stirrer is turned off. Reaction mixture (liquid layer without sediment) is decanted into a large beaker.
8. Pure distilled water 1 L is poured into the beaker and mix thoroughly.
9. A glycidate ester layer is separated down. Layers are separated with help of separatory funnel.

Note: Glycidate ester is used in following reactions without purification. If a chemist wants to use it as a product, he has to distill it from side reaction products due to an excess of ethyl 2-chloropropionate.​

​

BMK glycidic acid (sodium salt) synthesis BMK ethyl glycidate​

View attachment 16110​

10. Glycidic ester is loaded back into the clean reaction flask.​

11. The previously prepared and cooled NaOH sln. is poured into the drip funnel.
12. The stirrer is turned on. NaOH 30% aq. Solution 450 mL is slowly added to the reaction mixture. A reaction mixture temperature has to be maintained below <30°C.
13. Next, the reaction mixture is stirred for 12 h at room temperature.
14. After a while, distilled water 500 ml is added and the mixture is heated a little (no more than 60°C).
15. Benzene, toluene or other similar solvent 500 ml is poured into the heated reaction mixture.
16. The stirrer is turned off. The layers are formed.
17. With help of the separating funnel, the reaction by-products are extracted (not previously distilled ester by-products). The water layer with dissolved BMK glycidic acid (sodium salt) is separated back into the flask.

​

Phenylacetone (P2P) synthesis from BMK glycidic acid (sodium salt)​

View attachment 16111​

18. Using the drip funnel, concentrated (37%) aqueous hydrochloric acid (HCl) is carefully poured into the flask to reach pH1.​

19. The mixture is heated to 60°C and decarboxylated with constant stirring for 5 h.
20. Then, the stirrer is turned off and the mixture is separated into two layers. BMK layer is a top layer.

Note: If the mixture is cooled down, BMK layer will be at the bottom.

21. BMK layer is separated into a beaker using separatory funnel for further syntheses.

Note: After a while, remaining water in the beaker is completely separated from BMK oil.

BMK yield is ~300 ml (82%).​

G.Patton
Is the BMK glycidic acid (sodium salt) to water ratio 1:1 then add the hydrochloric acid to ph of 1?

View attachment 16107

This phenylacetone (P2P) synthesis approach is a simple way how to get phenylacetone from BMK ethyl glycidate and its synthesis from benzaldehyde. PMK ethyl glycidate can be hydrolyzed into P2P. This reaction isn't sensitive to water like BMK methyl glycidate synthesis. There is such advantage like a quite high yield conversion (82% from benzaldehyde to P2P). Moreover, the reaction doesn't take any elaborated equipment and can be easily scailed.​

Equipment and glassware:​

• Four necked round bottom reaction flask 3 L, equipped with reflux condenser, top stirrer and pressure equalized drip funnel 250 mL;​
• Funnel;​
• Retort stand and clamp for securing apparatus;​
• pH indicator paper;​
• Water/oil bath;​
• Retort stand and clamp for securing apparatus;​
• Laboratory grade thermometer (up to 10 - 100 °С);​
• Glass rod;​
• Silicone hoses;​
• Measuring cylinders for 100 mL and 1 L;​
• Laboratory scale (1-200 g is suitable);​
• Glass rod;​
• Beakers 3 L; 1 L x2; 500 ml x2;​
• Separatory funnel 2 L;​

Reagents:​

• Dimethylformamide 900 ml;​
• Benzaldehyde 300 ml;​
• Ethyl 2-chloropropionate 540 g;​
• Benzyltriethylammonium chloride (TEBAC) 32 g;​
• Potassium carbonate 780 g;​
• Sodium hydroxide (NaOH) 135 g;​
• Distilled water ~1.9 L;​
• Concentrated (37%) aqueous hydrochloric acid (HCl) ~250 mL;​

Download Video

Phenylacetone (P2P) Synthesis Via BMK Ethyl Glycidate

• Novator
• Jun 1, 2023
• 53
• 1-phenyl-2-propanone benzaldehyde bmk bmk ethyl glycidate bmk glycidic meth p2p synthesis

1) BMK ethyl glycidate synthesis from benzaldehyde.
2) BMK glycidic acid (sodium salt) synthesis...

​

BMK ethyl glycidate synthesis from benzaldehyde​

View attachment 16109 ​

1. Dimethylformamide 900 ml is poured into a 3 L four necked round bottom reaction flask, equipped with reflux condenser, top stirrer and drip funnel.​

2. Then, benzaldehyde 300 ml is added. A top stirrer is turned on.
3. Ethyl 2-chloropropionate 540 g is poured into the reactor. Benzyltriethylammonium chloride (TEBAC) catalyst 32 g is added. Next, potassium carbonate 780 g is added into the reaction mixture.
4. A heating of the water or oil bath is set at 40°C.
5. Reaction mixture is stirred for 48 h on the warm bath.
6. Sodium hydroxide (NaOH) 30% water solution 450 ml is prepared in advance.
7. After 48h, the stirrer is turned off. Reaction mixture (liquid layer without sediment) is decanted into a large beaker.
8. Pure distilled water 1 L is poured into the beaker and mix thoroughly.
9. A glycidate ester layer is separated down. Layers are separated with help of separatory funnel.

Note: Glycidate ester is used in following reactions without purification. If a chemist wants to use it as a product, he has to distill it from side reaction products due to an excess of ethyl 2-chloropropionate.​

​

BMK glycidic acid (sodium salt) synthesis BMK ethyl glycidate​

View attachment 16110​

10. Glycidic ester is loaded back into the clean reaction flask.​

11. The previously prepared and cooled NaOH sln. is poured into the drip funnel.
12. The stirrer is turned on. NaOH 30% aq. Solution 450 mL is slowly added to the reaction mixture. A reaction mixture temperature has to be maintained below <30°C.
13. Next, the reaction mixture is stirred for 12 h at room temperature.
14. After a while, distilled water 500 ml is added and the mixture is heated a little (no more than 60°C).
15. Benzene, toluene or other similar solvent 500 ml is poured into the heated reaction mixture.
16. The stirrer is turned off. The layers are formed.
17. With help of the separating funnel, the reaction by-products are extracted (not previously distilled ester by-products). The water layer with dissolved BMK glycidic acid (sodium salt) is separated back into the flask.

​

Phenylacetone (P2P) synthesis from BMK glycidic acid (sodium salt)​

View attachment 16111​

18. Using the drip funnel, concentrated (37%) aqueous hydrochloric acid (HCl) is carefully poured into the flask to reach pH1.​

19. The mixture is heated to 60°C and decarboxylated with constant stirring for 5 h.
20. Then, the stirrer is turned off and the mixture is separated into two layers. BMK layer is a top layer.

Note: If the mixture is cooled down, BMK layer will be at the bottom.

21. BMK layer is separated into a beaker using separatory funnel for further syntheses.

Note: After a while, remaining water in the beaker is completely separated from BMK oil.

BMK yield is ~300 ml (82%).​

if starting with BMK glycidic acid (sodium salt) is the ratio with water 1:1 then add the hydrochloric acid to ph of 1? then heat mixture and stir for 5hrs

 

[G.Patton]

Is the BMK glycidic acid (sodium salt) to water ratio 1:1 then add the hydrochloric acid to ph of 1?

if starting with BMK glycidic acid (sodium salt) is the ratio with water 1:1 then add the hydrochloric acid to ph of 1? then heat mixture and stir for 5hrs

rampage

Is the BMK glycidic acid (sodium salt) to water ratio 1:1 then add the hydrochloric acid to ph of 1?

Correct

 

[rampage]

Correct

G.Pattonfound this article, is 80 degrees to warm? is 1kg of hydrochloric acid too much just add to reach ph1?

How to convert BMK powder to oil?(Below is just a general description of hydrolysis process, you may still need to contact us if you cannot get oil properly.)
1,1kg powder mix with 1kg warm water (around 80 degrees).
2, put in 1kg hydrochloric acid (HCL 37%) and you will see bubble generated.
3,Stirring the mixture for one hour and then stop.
4,After one more hour you will get oil layer in light yellow color.
5,Use separate funnel to retrieve oil.

 

[rampage]

found this article, is 80 degrees to warm? is 1kg of hydrochloric acid too much just add to reach ph1?

How to convert BMK powder to oil?(Below is just a general description of hydrolysis process, you may still need to contact us if you cannot get oil properly.)
1,1kg powder mix with 1kg warm water (around 80 degrees).
2, put in 1kg hydrochloric acid (HCL 37%) and you will see bubble generated.
3,Stirring the mixture for one hour and then stop.
4,After one more hour you will get oil layer in light yellow color.
5,Use separate funnel to retrieve oil.

rampagehello
so as an example 1kg of bmk glycidic acid (sodium salt) and 1ltr of h2o are mixed, then hydrochloric acid is added to get a ph of 1.
then the rm is heated to 60 degrees and decarboxylated with constant stirring for 5hrs. then the heat and stirrer are turned off and the rm is transferred to a seperatory funnel where the layers are seperated.
top layer is p2p if the rm is still hot, or the bottom layer if rm is cold. so yield should be 1ltr of p2p?

 

[G.Patton]

hello
so as an example 1kg of bmk glycidic acid (sodium salt) and 1ltr of h2o are mixed, then hydrochloric acid is added to get a ph of 1.
then the rm is heated to 60 degrees and decarboxylated with constant stirring for 5hrs. then the heat and stirrer are turned off and the rm is transferred to a seperatory funnel where the layers are seperated.
top layer is p2p if the rm is still hot, or the bottom layer if rm is cold. so yield should be 1ltr of p2p?

rampage

so yield should be 1ltr of p2p?

No, ofc no. The yield about 70-85%.
Moles, grams, litres and chemical calculations There is explanation how to calculate it.

 

[chem19]

@G.Patton
In step 7 what should be pH of the layer separated?
as I had 2 samples, one freshly collected which has pH of 6 and is light in colour 600ml. While remaining 400 ml which was collected after 2 months from standing solution has pH of 8. And is about 400ml and slight dark in colour.
Which solution should I proceed with. Fresh one or later one, or both. Plz suggest. Looking for guidance. Thanks in advance.

 

[G.Patton]

@G.Patton
In step 7 what should be pH of the layer separated?
as I had 2 samples, one freshly collected which has pH of 6 and is light in colour 600ml. While remaining 400 ml which was collected after 2 months from standing solution has pH of 8. And is about 400ml and slight dark in colour.
Which solution should I proceed with. Fresh one or later one, or both. Plz suggest. Looking for guidance. Thanks in advance.

chem19First of all, I would like to say Hello.
Its pH is not important at stage 7. You can use both of them.

 

[chem19]

@G.Patton
In step 7 what should be pH of the layer separated?
as I had 2 samples, one freshly collected which has pH of 6 and is light in colour 600ml. While remaining 400 ml which was collected after 2 months from standing solution has pH of 8. And is about 400ml and slight dark in colour.
Which solution should I proceed with. Fresh one or later one, or both. Plz suggest. Looking for guidance. Thanks in advance.

chem19Here are the picture

 

[chem19]

@G.Patton hello,
Need your blessings and support.
In step 6 NaOH solution 30% 450 ml is required.
I have NaOH pellet. How much of these pellet are needed with how much water, to make desirable 450 ml solution.
Plz guide me, as I m getting different different answers.
Thanks in advance
Regards

 

[chem19]

@G.Patton hello,
Need your blessings and support.
In step 6 NaOH solution 30% 450 ml is required.
I have NaOH pellet. How much of these pellet are needed with how much water, to make desirable 450 ml solution.
Plz guide me, as I m getting different different answers.
Thanks in advance
Regards

chem19@G.Patton plz help me out, how to make 30% NaOH aq solution. Is it 30% w/w or w/c. Cauze chemicals are really costly, and a single wrong step may ruin whole process. Plz

 

[Throw-off]

@G.Patton plz help me out, how to make 30% NaOH aq solution. Is it 30% w/w or w/c. Cauze chemicals are really costly, and a single wrong step may ruin whole process. Plz

chem19Bro your over-thinking it. Look in Lab FAQ. Patton isn't gonna spoon feed you.

 

[chem19]

Bro your over-thinking it. Look in Lab FAQ. Patton isn't gonna spoon feed you.

Throw-off@Throw-off
Bro these are not hypothetical question, I m going through process, and these are refined problems that one who is going through wl face.
You just tell me in w/w and w/v, are you going to get same amount, huge difference,
Secondly after that to make pH 1 in another step while adding HCl is it not going to make difference. @G.Patton is here to guide us. So he will definitely going to spoon feed me and others. He is our mentor.
I m not arrogant, plz excuse me if you find so. But I m seriously looking for answer. I m in chemistry field from a long decade. So I know the importance of my questions. And this is not over thinking
Sorry if these text anyways made you think negative about me.

 

[Throw-off]

@Throw-off
Bro these are not hypothetical question, I m going through process, and these are refined problems that one who is going through wl face.
You just tell me in w/w and w/v, are you going to get same amount, huge difference,
Secondly after that to make pH 1 in another step while adding HCl is it not going to make difference. @G.Patton is here to guide us. So he will definitely going to spoon feed me and others. He is our mentor.
I m not arrogant, plz excuse me if you find so. But I m seriously looking for answer. I m in chemistry field from a long decade. So I know the importance of my questions. And this is not over thinking
Sorry if these text anyways made you think negative about me.

chem1930g of sodium hydroxide and 70ml H2o.

There is a massive difference between guide and the coddle you expect from him. I think your the first chemist who has been in the game for a decade who can't work out how to make a sodium hydroxide 30% solution? So Bravo give yourself a pat on the back. If you've got yourself in such a state from hydrolysis perhaps the real question you should be asking is "is this for you?".

 

[G.Patton]

@Throw-off
Bro these are not hypothetical question, I m going through process, and these are refined problems that one who is going through wl face.
You just tell me in w/w and w/v, are you going to get same amount, huge difference,
Secondly after that to make pH 1 in another step while adding HCl is it not going to make difference. @G.Patton is here to guide us. So he will definitely going to spoon feed me and others. He is our mentor.
I m not arrogant, plz excuse me if you find so. But I m seriously looking for answer. I m in chemistry field from a long decade. So I know the importance of my questions. And this is not over thinking
Sorry if these text anyways made you think negative about me.

chem19

You just tell me in w/w and w/v, are you going to get same amount, huge difference,

Water has 1g/1ml density, so that 1ml of distilled water can be counted as 1g.

 

[G.Patton]

@G.Patton hello,
Need your blessings and support.
In step 6 NaOH solution 30% 450 ml is required.
I have NaOH pellet. How much of these pellet are needed with how much water, to make desirable 450 ml solution.
Plz guide me, as I m getting different different answers.
Thanks in advance
Regards

chem19Hello
450*0.3=135g of NaOH is loaded into the beaker, add there water to reach 450 ml risk.

 

[Throw-off]

Anyone tried the new BMK Oil? cas 41232-97-7. A decade ago you could just get BMK powder make a solution with methanol 1:1 and drip it straight into the al/hg you would be done same day.. is hydrolysis required with all the new BMK derivatives? 5449 sodium salt sucks compared to the old school BMK.

 

[G.Patton]

Anyone tried the new BMK Oil? cas 41232-97-7. A decade ago you could just get BMK powder make a solution with methanol 1:1 and drip it straight into the al/hg you would be done same day.. is hydrolysis required with all the new BMK derivatives? 5449 sodium salt sucks compared to the old school BMK.

Throw-off

Anyone tried the new BMK Oil? cas 41232-97-7

You need to carry out alkaline hydrolysis and than acid one as for PMK glycidates.

A decade ago you could just get BMK powder make a solution with methanol 1:1 and drip it straight into the al/hg you would be done same day..

It isn't true, you couldn't make meth from BMK glycidic acid sodium salt directly. You need to get P2P at first.

 

[Throw-off]

You need to carry out alkaline hydrolysis and than acid one as for PMK glycidates.

It isn't true, you couldn't make meth from BMK glycidic acid sodium salt directly. You need to get P2P at first.

G.PattonI'm not saying it was a sodium salt, I know it wasn't a sodium salt the texture of the powder looked totally different consistency from BMK derivative 5449.