Phenylacetone (P2P) synthesis via BMK ethyl glycidate

G.Patton

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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;
  • pH indicator paper;
  • Water/oil bath;
  • 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

BMK ethyl glycidate synthesis from benzaldehyde

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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

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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)

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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%).
 

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Apparently, the best beema (brick-brick), probably the most convenient to buy water and increase the value at least 2 times more, and let the rest be taken care of by experts ;)
 

the money

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Thank you for your efforts
 

the money

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Thank you for writing the topic in detail and especially for always helping us to succeed, I really wish we had a video about the P2P synthesis of Benzaldehyde and Methyl ethyl ketone (MEK)

As you know anyone can supply methyl ethyl ketone (MEK) from stores and there is also a video for you on the synthesis of benzaldehyde
 

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Thank you for writing the topic in detail and especially for always helping us to succeed, I really wish we had a video about the P2P synthesis of Benzaldehyde and Methyl ethyl ketone (MEK)

As you know anyone can supply methyl ethyl ketone (MEK) from stores and there is also a video for you on the synthesis of benzaldehyde
the moneyBenzaldehyde isn't hard to synth and there's a few things on this site about it
 

btcboss2022

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Hello,
How many ml are aprox in the last water layer before HCL hydrolysis?And gr of sodium salt on it theoretically? Thanks.
 

G.Patton

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Hello,
How many ml are aprox in the last water layer before HCL hydrolysis?And gr of sodium salt on it theoretically? Thanks.
btcboss2022Hi, sorry for a long reply, haven't seen your question. About 1kg glycidate per 1 kg water. In case of 15% HCl acid, don't need dissolve in water at all. Don't overheat reaction, it's important.
 

chem19

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@G.Patton Ethyl 2-chloropropionate 540 g or 540 ml as it is available in liquid form commercially.and also in video there is liquid form poured.So plz advise.thanks in advance
 

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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;
  • pH indicator paper;
  • Water/oil bath;
  • 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

BMK ethyl glycidate synthesis from benzaldehyde

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

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)

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.PattonWhat screws me up is the visuals. I've only seen the ethyl glycidate as a white powder. So when I try to think how I would apply this process to that white powder (cas# 28578 16 7), I genuinely get confused. The worst part is that I feel like I should know the answer (considering my experience). I could see the powder melting to an oily substance (like what's seen in the video) when heated, but I believe the addition of 30% sodium hydroxide solution is done under 30 C... which I don't image is hot enough to melt said powder. So, how to (in my case) incorporate PMK Ethyl Glycidate (powder) cas# 28578 16 7) into this process? Maybe I'm just looking at this problem sideways, but I figure it's best if I just humble myself and ask for guidance at this point. So, anybody care to make me feel like a complete ass by pointing out the (most likely) obvious thing I'm missing, here?
 

G.Patton

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What screws me up is the visuals. I've only seen the ethyl glycidate as a white powder. So when I try to think how I would apply this process to that white powder (cas# 28578 16 7), I genuinely get confused. The worst part is that I feel like I should know the answer (considering my experience). I could see the powder melting to an oily substance (like what's seen in the video) when heated, but I believe the addition of 30% sodium hydroxide solution is done under 30 C... which I don't image is hot enough to melt said powder. So, how to (in my case) incorporate PMK Ethyl Glycidate (powder) cas# 28578 16 7) into this process? Maybe I'm just looking at this problem sideways, but I figure it's best if I just humble myself and ask for guidance at this point. So, anybody care to make me feel like a complete ass by pointing out the (most likely) obvious thing I'm missing, here?
Field7
cas# 28578 16 7
Hello, it is PMK ethyl glycidate, not BMK. BMK glycidic acid sodium salt has powdered form cas 5449-12-7.

Yes, you need heat your PMK up to 80*C. Look at appropriate topic please and continue your questions there if you won't find answers:
 

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Hello, it is PMK ethyl glycidate, not BMK. BMK glycidic acid sodium salt has powdered form cas 5449-12-7.

Yes, you need heat your PMK up to 80*C. Look at appropriate topic please and continue your questions there if you won't find answers:
G.PattonThat was quick reply. Thank you for that: it's much appreciated. Yeah, I do know the the difference between BMK and PMK. I know that can be used in the same reactions to get different end products (MDMA, Meth, MDA, amphet). I only used safrole as a starting point, but was considering PMK Ethyl Glycidate. Knowing the similarities, I was thinking I might use a portion of that (BMK) process on PMK E.G. to yield PMK. I was thinking a little outside the box, is all. I'll read the link you offered. Thanks, again.
 

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hello i have contacts with manufactures From whom i can source ephedrine powder and bmk CAS Number 5449-12-7 i have really good relationship with them for ephedrine it cost me $3500 per kg and for BMK it cost me $30 for kg i want to know which has the higest yield in terms of price and which is good for the quality

if i go throw via red P method for ephedrine and p2p to meth for bmk

also can i follow the same process like in this video if i have a complete powder form of ephedrine https://bbgate.com/media/methamphetamine-from-ephedrine-tablets-via-red-p.88/
ja1YYes I/rp, birch metod
 

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hello sir how i can convert BMK 5449-12-7 powder to liquid form and from where i can follow the process?
 

chem19

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@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.
 

G.Patton

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@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.
chem19about 10-15 min
 

jotoy

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@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?
 

bobbrown1488

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could you with 5449-12-7 powder at step 12 ?


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.
 

Beginner from China

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I would like to ask: Can Concentrated (37%) aqueous hydrochloric acid (HCl) be replaced by something else? Because I can’t buy it here
 

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I would like to ask: Can Concentrated (37%) aqueous hydrochloric acid (HCl) be replaced by something else? Because I can’t buy it here
Beginner from ChinaSulfuric acid and orthophosphoric. If not, you can take some other acids. It is not necessary to use 37% acid, you can take 15% and do not use additional water.
 
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