Phenylacetone (P2P) synthesis via BMK ethyl glycidate

chem19

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@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
 

G.Patton

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@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.
 

chem19

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Hello
450*0.3=135g of NaOH is loaded into the beaker, add there water to reach 450 ml risk.
G.Patton@G.Patton Thank you so much. You are best. God bless you. If I succeed i will definitely contribute to your bb project. I wish if I could be your experimental chemistry student. Thank you so much again.
 

Throw-off

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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

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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

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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.
 

guideme

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Hello experts, this is my first Post. Hope I will get response.
I got 200 ml glycidate ester
My question is how much sodium hydroxide solution,water and solvent should I use in step 11,14,15,
And HCl in step 18. Thanks
 

guideme

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Hello experts, this is my first Post. Hope I will get response.
I got 200 ml glycidate ester
My question is how much sodium hydroxide solution,water and solvent should I use in step 11,14,15,
And HCl in step 18. Thanks
guideme@G.Patton will I get a reply.i m noob. But I have chemical access
 
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guideme

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You can calculate them by yourself. It has a direct dependence and can be scaled down proportionately.
G.PattonG.Patton Plz correct me if I m wrong
For 700ml of Glycidic easter, you used 450 ml of 30% sodium hydroxide solution,
so for 200 ml I have to use 128.5 ml sodium hydroxide solution, and 142.8ml distilled water and 142.8 ml toulene.

Or if something else.plz notify me.
 

G.Patton

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G.Patton Plz correct me if I m wrong
For 700ml of Glycidic easter, you used 450 ml of 30% sodium hydroxide solution,
so for 200 ml I have to use 128.5 ml sodium hydroxide solution, and 142.8ml distilled water and 142.8 ml toulene.

Or if something else.plz notify me.
guidemeHow did you calculate 700ml number? From this batch, you'll get in theory 658ml of glycidic ester (100% yield). In a real synthesis it will be less.

so for 200 ml I have to use 128.5 ml sodium hydroxide solution, and 142.8ml distilled water and 142.8 ml toulene.
proportion is correct but you need to take not 700 ml. Count it for 530ml (for instance 80% yield).
 

panchaspsycho

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Hello experts, this is my first Post. Hope I will get response.
I got 200 ml glycidate ester
My question is how much sodium hydroxide solution,water and solvent should I use in step 11,14,15,
And HCl in step 18. Thanks
guidemeHCL addition is usually 2-3 times the amount of the glycidate powder or doing it by eye you add HCL slowly until it stops reacting with the water-glycidate solution.
 

chef learner

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Does the BMK oil=P2P produced using this process need to be further distilled and purified?
Or can you directly use BMK oil to make methamphetamine free base?
 

chef learner

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Is there any teacher who can answer this question? I need to clear up my doubts.

What is the quality of the P2P made using this method? I started with dimethylformamide, but according to the process and the teaching in the video, the color of my finished P2P seems to be very light. What is the reason for this and what will affect it? Will the results of the methamphetamine free base test be followed up?
 

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Throw-off

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Is there any teacher who can answer this question? I need to clear up my doubts.

What is the quality of the P2P made using this method? I started with dimethylformamide, but according to the process and the teaching in the video, the color of my finished P2P seems to be very light. What is the reason for this and what will affect it? Will the results of the methamphetamine free base test be followed up?
chef learnerIv had similar p2p surprise after hydrolysis too however mine was with poor quality BMK powder and the end product was quite weak.
 

Throw-off

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Is there any teacher who can answer this question? I need to clear up my doubts.

What is the quality of the P2P made using this method? I started with dimethylformamide, but according to the process and the teaching in the video, the color of my finished P2P seems to be very light. What is the reason for this and what will affect it? Will the results of the methamphetamine free base test be followed up?
chef learnerIv had similar p2p surprise after hydrolysis too however mine was with poor quality BMK powder and the end product was quite weak.
 

chef learner

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Iv had similar p2p surprise after hydrolysis too however mine was with poor quality BMK powder and the end product was quite weak.
Throw-offDoes every reagent used have a chance of affecting these? Or is there any reagent in the list that I need to replace?
I always use the same method, but this time it is different. It is obviously darker, but I don’t know which part affects it, because the time, quantity, and process are all the same.
 

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Throw-off

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Does every reagent used have a chance of affecting these? Or is there any reagent in the list that I need to replace?
I always use the same method, but this time it is different. It is obviously darker, but I don’t know which part affects it, because the time, quantity, and process are all the same.
chef learnerYour forgetting the main one that would effect it.. Temperature
 

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GPATTON just too be clear “19. The mixture is heated to 60°C and decarboxylated with constant stirring for 5 h.”
Is the mixture heated the whole time at 60 C or once it hits 60 C is the heat turned off with only constant stirring for 5 hours?? Thanks
 

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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.PattonI'm a little confused, this is BMK yield 300 ml, is it p2p or BMK oil
 

G.Patton

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I'm a little confused, this is BMK yield 300 ml, is it p2p or BMK oil
Manisj@1290What do you mean? BMK mean benzyl methyl ketone, that is the other name of phenyl-2-propanone (P2P). You can google it easy or open BB Wiki to read...
 
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