Reaktion #162262

Reaktionsgleichung

vinylphosphonic acid

methacrylic acid

AIBN

→

Vinylphosphonic Acid Methacrylic Acid

Lösungsmittel

ethyl acetate

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeIn a 10 liter flask equipped with a stirrer
2. 2
   workup.ADDITIONthe obtained solution was added dropwise in a reactor over 4 hours
3. 3
   workup.ADDITIONDuring the dropwise addition of a monomer solution
4. 4
   Sonstigea white precipitate was produced
5. 5
   TemperaturAfter heating
6. 6
   Temperaturwhile maintaining at 70° C.
7. 7
   Temperaturheating
8. 8
   Temperaturthe reaction solution was cooled to room temperature
9. 9
   SonstigeThe precipitate thus produced
10. 10
    Filtrationwas collected by filtration under reduced pressure
11. 11
    Waschenwashed with 1,000 g of ethyl acetate
12. 12
    SonstigeThe precipitate was vacuum-dried at 40° C. for 24 hours
13. 13
    Sonstigeto obtain a white fine crystal

Vorschrift

In a 10 liter flask equipped with a stirrer, a capacitor and a dropping device, 3,500 g of ethyl acetate was charged and heated to 70° C. Then, 390 g (3.61 mol) of a vinylphosphonic acid monomer, 1,243 g (14.44 mol) of methacrylic acid and 52 g of AIBN were dissolved in 1,000 g of ethyl acetate and the obtained solution was added dropwise in a reactor over 4 hours. During the dropwise addition of a monomer solution, a white precipitate was produced. After heating and stirring for 2 hours while maintaining at 70° C., heating was stopped and the reaction solution was cooled to room temperature. The precipitate thus produced was collected by filtration under reduced pressure and then washed with 1,000 g of ethyl acetate. The precipitate was vacuum-dried at 40° C. for 24 hours to obtain a white fine crystal. Yield: 1,550 g

Quelle