반응 #162262

반응 방정식

vinylphosphonic acid

methacrylic acid

AIBN

→

Vinylphosphonic Acid Methacrylic Acid

용매

ethyl acetate

ethyl acetate

반응 조건

후처리

1. 1
   기타In 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
   기타a white precipitate was produced
5. 5
   온도After heating
6. 6
   온도while maintaining at 70° C.
7. 7
   온도heating
8. 8
   온도the reaction solution was cooled to room temperature
9. 9
   기타The precipitate thus produced
10. 10
    여과was collected by filtration under reduced pressure
11. 11
    세척washed with 1,000 g of ethyl acetate
12. 12
    기타The precipitate was vacuum-dried at 40° C. for 24 hours
13. 13
    기타to obtain a white fine crystal

실험 절차

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

출처