تفاعل #2045083

معادلة التفاعل

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

المردود 73.1%

المذيبات

toluene

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe reaction mixture was extracted with dichloromethane
2. 2
   غسيلwashed with brine
3. 3
   تجفيفThe combined organic solutions were dried over Na2SO4
4. 4
   ترشيحfiltered
5. 5
   أخرىthe solvent was evaporated
6. 6
   أخرىto yield a crude product, which
7. 7
   أخرىwas recrystallized from DCM/hexane (1/1, v/v, 1200 mL)

الإجراء التجريبي

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.

المصدر