Σύνθεση γλυκιδικού άλατος BMK (άλας νατρίου) από βενζαλδεΰδη
- Thread starter G.Patton
- Start date
μπορεί να αντικατασταθεί το Methyl 2-chloropropionate;
- By G.Patton
Ναι, με αιθυλο-2-χλωροπροπιονικό, αλλά αυτή η αντίδραση είναι μεγαλύτερης διάρκειας.
- By virus0815
Γεια σας, ευχαριστώ πολύ για την απάντηση.
Παρόλο που η αντίδραση με το 2-χλωροπροπιονικό αιθύλιο διαρκεί περισσότερο, τουλάχιστον το 2-χλωροπροπιονικό αιθύλιο μπορεί να ληφθεί στο φόρουμ bbgate, οπότε αυτό θα χρησιμοποιήσω.
Πόσο αιθυλικό 2-χλωροπροπιονικό πρέπει να χρησιμοποιήσω; επίσης 350 g; πόσο περισσότερο χρόνο θα χρειαστεί περίπου η αντίδραση;
Παρόλο που η αντίδραση με το 2-χλωροπροπιονικό αιθύλιο διαρκεί περισσότερο, τουλάχιστον το 2-χλωροπροπιονικό αιθύλιο μπορεί να ληφθεί στο φόρουμ bbgate, οπότε αυτό θα χρησιμοποιήσω.
Πόσο αιθυλικό 2-χλωροπροπιονικό πρέπει να χρησιμοποιήσω; επίσης 350 g; πόσο περισσότερο χρόνο θα χρειαστεί περίπου η αντίδραση;
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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
Hello Sir:
I successfully made 5449 using the method in the post.
Then I made p2p.
Meth was made using sodium borohydride.
Customers reported that the effect of methamphetamine was very weak.
I want to know why.
The sodium salt obtained by this method was very wet. I had no way to dry it. I only used a Buchner funnel to filter out some of the water. I went directly to the next step of the reaction when the sodium salt was still very wet.
I used a small amount of water to dissolve the sodium salt, and then added 85% phosphoric acid. Probably because the sodium salt was not completely dried and contained a lot of water. The mixture could only be heated to about 100°. The mixture boiled very violently in the reactor. So much so that the coolant refrigeration device of the reflux condenser was heated to 60-70°. It was completely unable to cool a large amount of steam.
After about 6 hours of reflux, the heating was turned off and the mixture was allowed to separate into layers. The P2P obtained looked very dirty. I used steam to distill P2P. The distilled P2P was very yellow in color. In the distillation receiving bottle, P2P floated on the top layer, and the bottom layer was water. After cooling, all P2P was at the bottom layer, and the top layer was water. Does this P2P contain other substances that have not reacted completely? The P2P remaining in the distillation flask is very viscous.
What may be the cause of these problems?
I successfully made 5449 using the method in the post.
Then I made p2p.
Meth was made using sodium borohydride.
Customers reported that the effect of methamphetamine was very weak.
I want to know why.
The sodium salt obtained by this method was very wet. I had no way to dry it. I only used a Buchner funnel to filter out some of the water. I went directly to the next step of the reaction when the sodium salt was still very wet.
I used a small amount of water to dissolve the sodium salt, and then added 85% phosphoric acid. Probably because the sodium salt was not completely dried and contained a lot of water. The mixture could only be heated to about 100°. The mixture boiled very violently in the reactor. So much so that the coolant refrigeration device of the reflux condenser was heated to 60-70°. It was completely unable to cool a large amount of steam.
After about 6 hours of reflux, the heating was turned off and the mixture was allowed to separate into layers. The P2P obtained looked very dirty. I used steam to distill P2P. The distilled P2P was very yellow in color. In the distillation receiving bottle, P2P floated on the top layer, and the bottom layer was water. After cooling, all P2P was at the bottom layer, and the top layer was water. Does this P2P contain other substances that have not reacted completely? The P2P remaining in the distillation flask is very viscous.
What may be the cause of these problems?
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?
