反应详情

温度

90 °C

Under a nitrogen atmosphere, to a suspension of sodium hydride (60% in oil, 1.99 g) in THF (30 ml) was added a solution of the compound (6.90 g) obtained in step 2 in THF (20 mL) at 0° C., and the mixture was stirred at 90° C. for 1 hr. The reaction mixture was cooled to 10° C., and poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous ammonium chloride solution and brine, and concentrated. The residue was purified by silica gel column chromatography (solvent gradient; 10→66% ethyl acetate/hexane) to give the title compound (4.51 g, 75%) as a pale-yellow oil.

1. temperatureThe reaction mixture was cooled to 10° C.
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with saturated aqueous ammonium chloride solution and brine
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography (solvent gradient; 10→66% ethyl acetate/hexane)