HRID1037514

反应详情

EQUATION

反应方程式

HRID 1037514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 3,5-di(carbazol-9-yl)benzoate (1.0 g, 2.14 mmol) in THF/methanol (25.0 ml, 15:10) was added KOH (0.6 g, 10.69 mmol) in water (2.0 ml) at room temperature under stirring. The reaction was carried out at room temperature for 4.5 hours. The THF was evaporated. Next, methanol (20.0 ml) was added and then HCl water solution (80.0 ml; 15.0 ml of 36-38% HCl in 65.0 ml of water) was added. The mixture was stirred for 1 hour and a pale yellow solid product was obtained by filtration. The product was purified by recrystallization from acetone/water: 0.95 g (97.9%).

WORKUP

后处理

  1. customThe THF was evaporated
  2. additionNext, methanol (20.0 ml) was added
  3. additionHCl water solution (80.0 ml; 15.0 ml of 36-38% HCl in 65.0 ml of water) was added
  4. stirringThe mixture was stirred for 1 hour
  5. customa pale yellow solid product was obtained by filtration
  6. customThe product was purified by recrystallization from acetone/water