反应详情

温度

80 °C

To a solution of the product of Step 3, above (57) (1.85 mmol), in 2 ml DMF was added 60% sodium hydride in oil (3.6 mmol) at ambient temperature. The reaction mixture was stirred for 15 minutes and then 1,4-dibromobutane (1.85 mmol) was added. The reaction mixture was heated to 80° C. for 2 hours, cooled to ambient temperature, diluted with EtOAc and washed with saturated sodium bicarbonate and brine. The combined organics were then dried over MgSO4, filtered and concentrated to dryness. The crude material was chromatographed on silica gel using 10% EtOAc in hexanes as the eluant to obtain the title compound (58).

1. temperaturecooled to ambient temperature
2. washwashed with saturated sodium bicarbonate and brine
3. dry with materialThe combined organics were then dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. customThe crude material was chromatographed on silica gel using 10% EtOAc in hexanes as the eluant