反応 #162259

ord-ca6eee362d3d46539288822cee8c8317

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

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 ethanol
  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 ethanol was charged and heated to 70° C. Then, 720 g (6.67 mol) of a vinylphosphonic acid monomer, 880 g (12.38 mol) of acrylamide and 52 g of AIBN were dissolved in 1,000 g of ethanol 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 ethanol. The precipitate was vacuum-dried at 40° C. for 24 hours to obtain a white fine crystal. Yield: 1,550 g

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08835099B2uspto-grants-2014_09