HRID558042

反应详情

EQUATION

反应方程式

HRID 558042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In a 100-ml three-necked flask were placed 0.21 g (0.94 mmole) of palladium(II) acetate, 20 ml of xylene, and 0.76 g (3.76 mmoles) of tri-tert-butylphosphine and the mixture was heated at 60° C. with stirring for 30 minutes. The resulting solution was sent into a solution that had been prepared by dissolving 4.61 g (0.0180 mole) of indolo[2,3-a]carbazole, 5.8 g (0.018 mole) of 4-carbazolylbromobenzene, and 7.7 g (0.080 mole) of sodium tert-butoxide in 180 ml of xylene and heated at 60° C. in a stream of nitrogen and the combined solution was heated up to 130° C. and kept at this temperature for 5 hours with stirring. The solution was cooled to room temperature, 200 ml of water was added, and the organic layer was separated and concentrated under reduced pressure to give a crude product. The crude product was purified by crystallization from dichloromethane and ethanol, the solvent was distilled off under reduced pressure, and 4.2 g (0.0084 mole, 47% yield) of 11-(4-carbazolylphenyl)indolo[2,3-a]carbazole was obtained.

WORKUP

后处理

  1. customIn a 100-ml three-necked flask were placed
  2. customhad been prepared
  3. temperaturethe combined solution was heated up to 130° C.
  4. waitkept at this temperature for 5 hours
  5. stirringwith stirring
  6. temperatureThe solution was cooled to room temperature
  7. customthe organic layer was separated
  8. concentrationconcentrated under reduced pressure
  9. customto give a crude product
  10. customThe crude product was purified by crystallization from dichloromethane and ethanol
  11. distillationthe solvent was distilled off under reduced pressure