反应详情

To a solution of 93 (300 mg, 0.84 mmol) in dry DMF (3 ml) at 0° C. was added NaH (40 mg, 60% dispersion in oil, 1.0 mmol). The mixture was allowed to warm to room temperature over 0.5 h then re-cooled to 0° C. Bromoethylmethyl ether (123 mg, 0.88 mmol) was added and mixture was allowed to warm to room temperature over 20 hours, concentrated and partitioned between EtOAc and water. The EtOAc phase was dried over anhydrous Na2SO4, filtered, concentrated and purified by column chromatography (eluents hexane and acetone/hexane 75:25) to afford the title compound 94 (126 mg, 36% yield) as a pale yellow solid. MS (m/z) 415.1.0 (M+H).

1. temperaturethen re-cooled to 0° C
2. temperatureto warm to room temperature over 20 hours
3. concentrationconcentrated
4. custompartitioned between EtOAc and water
5. dry with materialThe EtOAc phase was dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified by column chromatography (eluents hexane and acetone/hexane 75:25)