反应详情

温度

-78 °C

To a solution of 4′,4-dibromobiphenyl (3.12 g, 10 mmol) in dry THF (50 mL) at −78° C. was added dropwise a solution of n-BuLi (1.6M in hexane, 10 mmol). After addition, the mixture was stirred for 30 minutes at −78° C. Anhydrous DMF (50 mL) was then added and the mixture was allowed to stir at room temperature for 2 hours. The solvent was removed under high vacuum and the residue was taken in water and extracted with dichloromethane (2×50 mL). The combined organic layer were dried (MgSO4) and concentrated. Purification by flash chromatography (ethyl acetate/hexane: 2/8) gave the title compound 152 55% yield. MS (ESI)=261 (MH+).

1. additionAfter addition
2. stirringto stir at room temperature for 2 hours
3. customThe solvent was removed under high vacuum
4. extractionextracted with dichloromethane (2×50 mL)
5. dry with materialThe combined organic layer were dried (MgSO4)
6. concentrationconcentrated
7. customPurification by flash chromatography (ethyl acetate/hexane: 2/8)