BMK Glycidate Sodium Salt Synthesis
- Thread starter G.Patton
- Start date
Může být methyl 2-chlorpropionát nahrazen?
Long time no see, sir: Since 5449 is not available now, I am considering a new way to make P2P.
If I start from 14 and add 1:1 phosphoric acid to start the reaction, can I get P2P? Before that, is there anything else I need to do?
Or do I have to add sodium hydroxide solution first, cool and crystallize to get 5449. Then react with phosphoric acid to get P2P?
I have seen another link, and it may be due to translation reasons, the names of many chemical substances are different, and I can't be sure. If you can give me an answer, I would be very grateful!
If I start from 14 and add 1:1 phosphoric acid to start the reaction, can I get P2P? Before that, is there anything else I need to do?
Or do I have to add sodium hydroxide solution first, cool and crystallize to get 5449. Then react with phosphoric acid to get P2P?
I have seen another link, and it may be due to translation reasons, the names of many chemical substances are different, and I can't be sure. If you can give me an answer, I would be very grateful!
- By G.Patton
What is 14? Can you name substances in accordance with IUPAC or their CAS? I don't understand you.
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- By qwe111
Sorry sir,
I quoted the part from your post but the website does not show it.
13. The stirrer is turned off. RM is separated into two layers. The top layer is methyl glycidic ester (BMK methyl glycidate), the lower layer is water with unnecessary reaction salts, which are dissolved in it. The lower layer is discarded, the top glycidic ester layer is used in the further reactions.
14. BMK-glycidate methyl ester is left in the reactor. It can be vacuum distilled to produce the purer ester in case you want to sale it as a product. Approximate ester amount is around 400 g. As an option, the ester is used in the next reaction to obtain the sodium or potassium salt of glycidic acid.
At this point in the experiment, the water layer is discarded and the upper oil layer (glycidyl esters) is retained.
I want to get P2P. Add phosphoric acid to the retained oil layer and heat it under reflux for 4-6 hours. Is this correct?
Or do I need to do something else before I add phosphoric acid?
I quoted the part from your post but the website does not show it.
13. The stirrer is turned off. RM is separated into two layers. The top layer is methyl glycidic ester (BMK methyl glycidate), the lower layer is water with unnecessary reaction salts, which are dissolved in it. The lower layer is discarded, the top glycidic ester layer is used in the further reactions.
14. BMK-glycidate methyl ester is left in the reactor. It can be vacuum distilled to produce the purer ester in case you want to sale it as a product. Approximate ester amount is around 400 g. As an option, the ester is used in the next reaction to obtain the sodium or potassium salt of glycidic acid.
At this point in the experiment, the water layer is discarded and the upper oil layer (glycidyl esters) is retained.
I want to get P2P. Add phosphoric acid to the retained oil layer and heat it under reflux for 4-6 hours. Is this correct?
Or do I need to do something else before I add phosphoric acid?
- By G.Patton
Hello.
No, it is not correct. You have to follow steps in the P2P synthesis from BMK glycidate ethers tutorial.
No, it is not correct. You have to follow steps in the P2P synthesis from BMK glycidate ethers tutorial.
- By qwe111
14. BMK-glycidate methyl ester is left in the reactor. It can be vacuum distilled to produce the purer ester in case you want to sale it as a product. Approximate ester amount is around 400 g. As an option, the ester is used in the next reaction to obtain the sodium or potassium salt of glycidic acid.
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. ..........
14. ......。
15. Benzene, toluene or other similar solvent 500 ml is poured into the heated reaction mixture.
16. .......
17.......。
Hello sir: According to my understanding, start from step 14 of this article, and then proceed from step 10 of another article to step 17. Get the water layer containing sodium salt.
It seems that phosphoric acid can be added to react next?
In step 12, stirring at room temperature for 12 hours, can it be replaced by heating for 1 hour?
In step 15, can the benzene and toluene used be replaced by dichloromethane, ethyl acetate, or petroleum ether?
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. ..........
14. ......。
15. Benzene, toluene or other similar solvent 500 ml is poured into the heated reaction mixture.
16. .......
17.......。
Hello sir: According to my understanding, start from step 14 of this article, and then proceed from step 10 of another article to step 17. Get the water layer containing sodium salt.
It seems that phosphoric acid can be added to react next?
In step 12, stirring at room temperature for 12 hours, can it be replaced by heating for 1 hour?
In step 15, can the benzene and toluene used be replaced by dichloromethane, ethyl acetate, or petroleum ether?
- By qwe111
Hi Sir,
Of course I know about racemic and D-meth.
I have done tartaric acid separation of isomers and obtained pure D-meth, but the customer feedback said that the effect was poor.
I used 5449 purchased from the manufacturer before, and the P2P obtained by the reaction was very clean after distillation, almost transparent white.
The D-meth was very effective.
This time all other reagents used were the same, only 5449 was different.
I am not sure whether P2P contains unreacted benzaldehyde or methyl 2-chloropropionate.
I want to try to use other methods to clean P2P to remove the benzaldehyde or methyl 2-chloropropionate contained in it, but so far, I have not found any useful answers.
Sir, do you know any effective methods?
Happy New Year!
Of course I know about racemic and D-meth.
I have done tartaric acid separation of isomers and obtained pure D-meth, but the customer feedback said that the effect was poor.
I used 5449 purchased from the manufacturer before, and the P2P obtained by the reaction was very clean after distillation, almost transparent white.
The D-meth was very effective.
This time all other reagents used were the same, only 5449 was different.
I am not sure whether P2P contains unreacted benzaldehyde or methyl 2-chloropropionate.
I want to try to use other methods to clean P2P to remove the benzaldehyde or methyl 2-chloropropionate contained in it, but so far, I have not found any useful answers.
Sir, do you know any effective methods?
Happy New Year!
- By G.Patton
Hi. Let anyone else check it. Probably it's his subjective opinion.
Distillation is effective enough method. Also, you can use bisulfite purification. But in my opinion, it's excessive and has no reason to do (in your case).
Distillation is effective enough method. Also, you can use bisulfite purification. But in my opinion, it's excessive and has no reason to do (in your case).
Other metal alcoholates such as sodium methoxide, potassium tert-butoxide, sodium isopropoxide, etc. can be used. In addition, sodium hydride, sodium amide can be used as well. RM is heated up and thickened a little during the EtONa addition, an external cooling is applied.
Other metal alcoholates such as sodium methoxide, potassium tert-butoxide, sodium isopropoxide, etc. can be used. In addition, sodium hydride, sodium amide can be used as well. RM is heated up and thickened a little during the EtONa addition, an external cooling is applied.
Hello sir,
Any of these reagents can be used in place of sodium ethoxide?
Other metal alcoholates such as sodium methoxide, potassium tert-butoxide, sodium isopropoxide, etc. can be used. In addition, sodium hydride, sodium amide can be used as well. RM is heated up and thickened a little during the EtONa addition, an external cooling is applied.
Hello sir,
Any of these reagents can be used in place of sodium ethoxide?
