Syntese af BMK-glycidat (natriumsalt) fra benzaldehyd

haze2000

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Junglemetoden (HDPE-tønder) fungerer ikke med denne procedure på grund af vandspor?
 

G.Patton

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Sandsynligvis ja. Jeg er ikke sikker på, hvilken tilstand du taler om.
 

G.Patton

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Hvad mener du? Hvad mener du med det? HDPE er plastik. Hvordan kan det være hygroskopisk?
 

jasper

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Er der nogen erstatning? Af methyl 2-chlorpropionat?
 

virus0815

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Kan Methyl 2-chloropropionat erstattes?
 

G.Patton

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Ja, med ethyl 2-chlorpropionat, men denne reaktion er længere.
 

virus0815

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Hej, mange tak for svaret.
Selvom reaktionen med ethyl 2-chlorpropionat tager længere tid, kan man i det mindste få ethyl 2-chlorpropionat på bbgate-forummet, så det er den, jeg vil bruge.
hvor meget ethyl 2-chloropropionat skal jeg bruge? også 350 g? hvor meget længere ville reaktionen cirka tage?
 
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G.Patton

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Hej, samme molære ækvivalent.
Brug bare præcis EtONa på dette trin. Det andet er det samme.
8. Når RM er kølet ned til 0°С inde i reaktoren, påbegyndes tilsætning af 200 g tørt natriumethylat (EtONa).
 

haze2000

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Kan en HDPE-tønde (200L) bruges til denne reaktion?
 

should

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Can the residue in the final flask be mixed with the finished product in the receiving bottle for use?
 

qwe111

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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!
 

G.Patton

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What is 14? Can you name substances in accordance with IUPAC or their CAS? I don't understand you.
 
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qwe111

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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?
 

qwe111

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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?
 

G.Patton

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I sent you link above, you have to start from the first step. You can substitute step with HCl by H3PO4.
 
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