HRID1263051

反应详情

EQUATION

反应方程式

HRID 1263051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

16.7 g (0.1 mole) of 2,3-dichloromaleic anhydride is dissolved in 100 ml of dioxane, and a solution of 15.9 g (0.1 mole) of o-difluoromethoxyaniline in 30 ml of dioxane is added dropwise to it at room temperature over 20 minutes with stirring. Thereafter, the resulting solution is stirred at 70°-80° C. for 2 hours and the dioxane is then distilled off under a reduced pressure. Water is added to the residue to precipitate crystals. The precipitated crystals are filtered off and recrystallized from ethanol to give 27.7 g (yield: 90%) of 2,3-dichloro-N-(o-difluoromethoxyphenyl)maleimide melting at 103.5°-104° C. in the form of light yellow crystals.

WORKUP

后处理

  1. stirringThereafter, the resulting solution is stirred at 70°-80° C. for 2 hours
  2. distillationthe dioxane is then distilled off under a reduced pressure
  3. additionWater is added to the residue
  4. customto precipitate crystals
  5. filtrationThe precipitated crystals are filtered off
  6. customrecrystallized from ethanol