反应详情

To a solution of product of Step 4, above (58) (1.0 mmol) in 2 ml CCl4 was added bromine (1.0 mmol) at ambient temperature and the reaction mixture was stirred for 2 hours, refluxed for 1 hour to ensure completion of the reaction, cooled to ambient temperature, diluted with CH2 Cl2 and washed with saturated sodium bicarbonate and brine. The combined organics were dried over MgSO4, filtered and concentrated to dryness. The crude residue was chromatographed on silica gel using 5% EtOAc in hexanes as the eluant to obtain the title compound (59).

1. temperaturerefluxed for 1 hour
2. customcompletion of the reaction
3. washwashed with saturated sodium bicarbonate and brine
4. dry with materialThe combined organics were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated to dryness
7. customThe crude residue was chromatographed on silica gel using 5% EtOAc in hexanes as the eluant