反应详情

温度

-40 °C

A 2.5M solution of butyllithium in hexanes (1.8 eq), (Aldrich) was added dropwise to a solution of 1-bromo-3-chlorobenzene (1.5 eq) in anhydrous diethyl ether with stirring under argon at -40° C. After stirring at room temperature for 0.5 h, a solution of 9-fluorenone (1 eq), (Aldrich) in anhydrous diethyl ether was added dropwise to the mixture with stirring and cooling at 0° C. The reaction mixture was stirred at room temperature for 1 h, poured into a saturated solution of ammonium chloride and extracted with dichloromethane. The combined dichloromethane extracts were washed with brine, dried (MgSO4), the solvent evaporated and the residue chromatographed on silica gel column with 10% ethyl acetate in hexanes to give the title compound as an oil.

1. stirringAfter stirring at room temperature for 0.5 h
2. stirringwith stirring
3. temperaturecooling at 0° C
4. stirringThe reaction mixture was stirred at room temperature for 1 h
5. extractionextracted with dichloromethane
6. washThe combined dichloromethane extracts were washed with brine
7. dry with materialdried (MgSO4)
8. customthe solvent evaporated
9. customthe residue chromatographed on silica gel column with 10% ethyl acetate in hexanes