反応 #162262

反応方程式

vinylphosphonic acid

methacrylic acid

AIBN

→

Vinylphosphonic Acid Methacrylic Acid

溶媒

ethyl acetate

ethyl acetate

反応条件

後処理

1. 1
   その他In 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
   その他a white precipitate was produced
5. 5
   温度After heating
6. 6
   温度while maintaining at 70° C.
7. 7
   温度heating
8. 8
   温度the reaction solution was cooled to room temperature
9. 9
   その他The precipitate thus produced
10. 10
    ろ過was collected by filtration under reduced pressure
11. 11
    洗浄washed with 1,000 g of ethyl acetate
12. 12
    その他The precipitate was vacuum-dried at 40° C. for 24 hours
13. 13
    その他to obtain a white fine crystal

実験手順

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

出典