反应详情

To a stirred solution of compound (15) (1 g, 2.7 mmol) in acetonitrile (10 mL) under nitrogen was added (10 mg, 0.008 mmol) of tetrakis(triphenylphosphine) palladium (0) followed by morpholine (0.28 mL, 0.28 g, 3.2 mmol). After one hour, the solvent was removed in vacuo. The resulting oil was dissolved in diethyl ether (50 mL) and the organic phase was washed with 2N HCl (20 mL), water (20 mL) and brine (20 mL). The ether layer was dried over anhydrous sodium sulfate and concentrated to give an oil, which was purified by column chromatography on silica gel, eluting with 30% ethyl acetate:hexane. The desired product (11) was isolated as a white crystalline solid (0.75 g, 84% yield), m.p 63-64° C.

1. customthe solvent was removed in vacuo
2. dissolutionThe resulting oil was dissolved in diethyl ether (50 mL)
3. washthe organic phase was washed with 2N HCl (20 mL), water (20 mL) and brine (20 mL)
4. dry with materialThe ether layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customto give an oil, which
7. customwas purified by column chromatography on silica gel
8. washeluting with 30% ethyl acetate