BMK Glycidate Sodium Salt Synthesis

haze2000

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Džiunglių metodas ( HDPE statinės) neveikia su šia procedūra dėl vandens pėdsakų?
 

G.Patton

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Tikėtina, kad taip. Nesu tikras, apie kokią sąlygą kalbate.
 

G.Patton

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Ką? Ką jūs turite omenyje? HDPE yra plastikas. Kaip jis gali būti higroskopiškas?
 

jasper

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Ar yra koks nors jų pakaitalas? Metilo 2-chloropropionato?
 
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Ar galima pakeisti metilo 2-chloropropionatą?
 

G.Patton

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Taip, etilo 2-chlorpropionatu, tačiau ši reakcija yra ilgesnė.
 
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Sveiki, labai ačiū už atsakymą.
nors reakcija su etil 2-chlorpropionatu trunka ilgiau, bent jau etil 2-chlorpropionato galima gauti bbgate forume, todėl būtent jį ir naudosiu
kiek etil 2-chlorpropionato turėčiau naudoti? taip pat 350 g? kiek laiko maždaug užtruktų reakcija?
 
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G.Patton

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Sveiki, tas pats molinis ekvivalentas.
Tiesiog šiame etape vartokite būtent EtONą. Kitaip yra tas pats.
8. Kai RM reaktoriaus viduje atšaldomas iki 0°С, pradedamas sauso natrio etilato 200 g (EtONa) pridėjimas.
 

haze2000

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Ar šiai reakcijai galima naudoti HDPE statinę (200 l)?
 

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?
 

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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.
 

qwe111

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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!
 

G.Patton

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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).
 

Manisj@1290

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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?
 

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Hello, exactly.
 

The Silent Chemist

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so lithium ethoxide can be used ?, I ask this because lithium is commonly available apposed to sodium or potassium and one could synthesize there own lithium ethoxide quite easily
 

G.Patton

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I guess so.
 
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