Σύνθεση γλυκιδικού άλατος BMK (άλας νατρίου) από βενζαλδεΰδη

[haze2000]

Η μέθοδος Jungle ( βαρέλια HDPE) δεν θα λειτουργήσει με αυτή τη διαδικασία λόγω των ιχνών νερού;

 

[G.Patton]

Πιθανώς ναι. Δεν είμαι σίγουρος για ποια κατάσταση μιλάτε.

 

[G.Patton]

Τι; Τι εννοείτε; Το HDPE είναι πλαστικό. Πώς μπορεί να είναι υγροσκοπικό;

 

[jasper]

Υπάρχει κάποιο υποκατάστατό τους; του 2-χλωροπροπιονικού μεθυλίου;

 

[virus0815]

μπορεί να αντικατασταθεί το Methyl 2-chloropropionate;

 

[G.Patton]

Ναι, με αιθυλο-2-χλωροπροπιονικό, αλλά αυτή η αντίδραση είναι μεγαλύτερης διάρκειας.

 

[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;

 

[G.Patton]

hi, ίδιο μοριακό ισοδύναμο.
Απλά χρησιμοποιήστε ακριβώς EtONa σε αυτό το στάδιο. Το άλλο είναι το ίδιο.
8. Όταν το RM ψύχεται στους 0°С μέσα στον αντιδραστήρα, αρχίζει η προσθήκη ξηρού αιθυλικού νατρίου 200 g (EtONa).

 

[haze2000]

Μπορεί να χρησιμοποιηθεί βαρέλι HDPE (200L) για αυτή την αντίδραση;

 

[G.Patton]

Ναι

 

[should]

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

 

[qwe111]

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!

 

[qwe111]

• G.Patton

 

[G.Patton]

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

 

[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?

 

[G.Patton]

Hello.
No, it is not correct. You have to follow steps in the P2P synthesis from BMK glycidate ethers tutorial.

 

[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?

 

[G.Patton]

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