HRID531897

反应详情

EQUATION

反应方程式

HRID 531897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
144 °C

PROCEDURE

实验过程

25 g (96.6 mmol) of 11,12-dihydroindolo[2,3-a]carbazole are added to 12.5 g (48 mmol) of 2-iodobenzenethiol in 80 ml of di-n-butyl ether, and the solution is degassed. 6.6 g (0.105 mmol) of copper powder, 0.92 g (0.003 mmol) of copper(I) iodide and 14.6 g (106.6 mmol) of K2CO3 are subsequently added to the mixture, which is then stirred at 144° C. under protective gas for 4 days. The organic phase is dried over MgSO4, and the solvent is removed in vacuo. The residue is recrystallised from acetone and finally sublimed in a high vacuum. Yield: 22.5 g (61 mmol), 66% of theory, purity according to HPLC 89.4%.

WORKUP

后处理

  1. customthe solution is degassed
  2. dry with materialThe organic phase is dried over MgSO4
  3. customthe solvent is removed in vacuo
  4. customThe residue is recrystallised from acetone