反应详情

温度

60 °C

In a 100-ml three-necked flask that had been deaerated and filled with nitrogen was placed a solution of 0.21 g (0.94 millimole) of palladium(II) acetate, 0.76 g (3.8 millimoles) of tri-tert-butylphosphine was added, and the mixture was heated at 60° C. with stirring for 30 minutes. The resulting solution was transferred under nitrogen flow to a solution heated at 60° C. of 4.6 g (18.0 millimoles) of indolo[2,3-a]carbazole, 5.8 g (18.0 millimoles) of 3-carbazolylbromobenzene, and 7.7 g (80.0 millimoles) of sodium tert-butoxide in 180 ml of xylene. The solution was then heated to 130° C., and heated with stirring at this temperature for 5 hours. The solution was cooled to room temperature and 200 ml of water was added. The mixture was subjected to oil-water separation, and the organic layer was concentrated under reduced pressure to give a crude product. The crude product was purified by crystallization from dichloromethane and ethanol, the solvent was stripped off under reduced pressure, and 4.2 g (8.4 millimoles, 47% yield) of 11-(4-carbazolylphenyl)indolo[2,3-a]carbazole was obtained.

1. customIn a 100-ml three-necked flask that had been deaerated
2. additionfilled with nitrogen
3. additionwas added
4. temperatureThe solution was then heated to 130° C.
5. temperatureheated
6. stirringwith stirring at this temperature for 5 hours
7. temperatureThe solution was cooled to room temperature
8. customThe mixture was subjected to oil-water separation
9. concentrationthe organic layer was concentrated under reduced pressure
10. customto give a crude product
11. customThe crude product was purified by crystallization from dichloromethane and ethanol