反应 #2045083

反应方程式

3-bromo-9H-carbazole

9-phenyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-9H-carbazole

K3PO4

→

9H,9′H-3,3′-bicarbazole

收率 73.1%

溶剂

toluene

water

反应条件

后处理

1. 1
   萃取the reaction mixture was extracted with dichloromethane
2. 2
   洗涤washed with brine
3. 3
   干燥The combined organic solutions were dried over Na2SO4
4. 4
   过滤filtered
5. 5
   其他the solvent was evaporated
6. 6
   其他to yield a crude product, which
7. 7
   其他was recrystallized from DCM/hexane (1/1, v/v, 1200 mL)

实验过程

A mixture solution of 3-bromo-9H-carbazole (6.75 g, 27.4 mmol), 9-phenyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-9H-carbazole (12.15 g, 32.9 mmol), Pd2(dba)3 (0.251 g, 0.274 mmol), SPhos (0.450 g, 1.097 mmol) and K3PO4 (25.3 g, 110 mmol) in toluene (500 mL) and water (50 mL) was refluxed under nitrogen for 10 h. After cooling to room temperature, the reaction mixture was extracted with dichloromethane and washed with brine. The combined organic solutions were dried over Na2SO4, filtered, and the solvent was evaporated to yield a crude product, which was recrystallized from DCM/hexane (1/1, v/v, 1200 mL) to yield 9H,9′H-3,3′-bicarbazole (6.66 g, 59%) as a yellow solid.

来源