HRID1672115

反应详情

EQUATION

反应方程式

HRID 1672115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a flask, 30 g of 4-hydroxyphenyldiphenylsulfonium perfluorobutanesulfonate and 300 g of dichloromethane were added to prepare a solution. In the flask, a nitrogen gas was blown. To the solution, 17.9 g of N,N-diethylcarbamoyl chloride was added and then 10.5 g of triethylamine was added thereto. The resultant mixture was stirred at room temperature for 1 hour. To the obtained reaction mixture, 100 g of ion-exchanged water was added and an organic layer was obtained by separation. The obtained organic layer was washed with 300 mL of distillated water and then dried over anhydrous magnesium sulfate. Magnesium sulfate was removed by filtration and the obtained filtrate was concentrated. The obtained residue was dried under reduced pressure to obtain 26.7 g of 4-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonate.

WORKUP

后处理

  1. customto prepare a solution
  2. additionwas added
  3. customan organic layer was obtained by separation
  4. washThe obtained organic layer was washed with 300 mL of distillated water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customMagnesium sulfate was removed by filtration
  7. concentrationthe obtained filtrate was concentrated
  8. customThe obtained residue was dried under reduced pressure