HRID363279

反应详情

EQUATION

反应方程式

HRID 363279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

67.0 g (0.37 mol) of 9-methylcarbazole were dissolved in 400 ml of dry dichloroethane, to which 105.0 g (0.79 mol) of AlCl3 were added. 104.0 g (0.74 mol) of benzoyl chloride were added dropwise with stirring and cooling with ice. Stirring was continued for another 3 hours at room temperature, and the reaction mixture was then decomposed with ice and hydrochloric acid and the organic phase was washed to neutrality with water and NaHCO3 solution. The remaining water was removed by azeotropic distillation. The dichloroethane solution was concentrated, whereupon the diketone crystallized out. It was recrystallized once more from dichloroethane; m.p. 222° C.; (Lit. 16): m.p. 2190° C.), colorless crystals. Yield: 114.2 g (79.3%).

WORKUP

后处理

  1. additionwere added
  2. temperaturecooling with ice
  3. stirringStirring
  4. washthe organic phase was washed
  5. customThe remaining water was removed by azeotropic distillation
  6. concentrationThe dichloroethane solution was concentrated, whereupon the diketone
  7. customcrystallized out
  8. customIt was recrystallized once more from dichloroethane