反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 160 °C
PROCEDURE
实验过程
A mixture of 10.9 g (35.1 mmol) 4-iododibenzo[b,d]thiophene, 8.6 g (35.1 mmol) of 3-bromo-9H-carbazole, 4.46 g (70.2 mmol) of Cu, 14.55 g (100.1 mmole) of K2CO3 was stirred in 100 ml dimethylformamide, the reaction mixture was then heat to 160° C. for about overnight under nitrogen. Then cooled to 100° C., the solution was filtered. To receive the filtrate, and most of the dimethylformamide was removed under reduced pressure from the filtrate. The distillation was extracted with ethyl acetate and water, dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica(hexane-dichloromethane) to give product 8.7 g (58%).
WORKUP
后处理
- temperatureThen cooled to 100° C.
- filtrationthe solution was filtered
- custommost of the dimethylformamide was removed under reduced pressure from the filtrate
- distillationThe distillation
- extractionwas extracted with ethyl acetate and water
- dry with materialdried with anhydrous magnesium sulfate
- customthe solvent was removed
- customthe residue was purified by column chromatography on silica(hexane-dichloromethane)