반응 #2045083

반응 방정식

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

수율 73.1%

용매

toluene

water

반응 조건

후처리

1. 1
   추출the reaction mixture was extracted with dichloromethane
2. 2
   세척washed with brine
3. 3
   건조The combined organic solutions were dried over Na2SO4
4. 4
   여과filtered
5. 5
   기타the solvent was evaporated
6. 6
   기타to yield a crude product, which
7. 7
   기타was recrystallized from DCM/hexane (1/1, v/v, 1200 mL)

실험 절차

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.

출처