HRID1516998

反应详情

EQUATION

反应方程式

HRID 1516998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 4-bromodibenzo[b,d]thiophene (2.061 g, 7.83 mmol), 9-phenyl-9H,9′H-3,3′-bicarbazole (2 g, 4.90 mmol), and sodium t-butoxide (1.412 g, 14.69 mmol) in 200 mL of xylene was bubbled with N2 for 20 min. Pd2(dba)3 (0.045 g, 0.049 mmol) and dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (0.080 g, 0.196 mmol) were added and bubbled with nitrogen for another 20 min, then the mixture was heated to reflux under N2 for 24 h. The mixture was cooled and filtered through Celite. After solvent evaporation, the residue was coated on Celite and purified by column chromatography using 2:3 dichloromethane and hexanes as solvent. 9-(dibenzo[b,d]thiophen-4-yl)-9′-phenyl-9H,9′H-3,3′-bicarbazole (2.2 g. 3.72 mmol, 76% yield) was obtained. The product was further purified by recrystallization with dichloromethane and hexane.

WORKUP

后处理

  1. customwas bubbled with N2 for 20 min
  2. custombubbled with nitrogen for another 20 min
  3. temperaturethe mixture was heated
  4. temperatureto reflux under N2 for 24 h
  5. temperatureThe mixture was cooled
  6. filtrationfiltered through Celite
  7. customAfter solvent evaporation
  8. custompurified by column chromatography