反应详情

To a stirred solution of compound (15) (1 g, 2.7 mmol) in dioxane (9 mL) was added ammonium formate (341 mg, 2.7 mmol) and palladium(II) acetate (12 mg) under a nitrogen atmosphere. The reaction mixture was heated to reflux for one hour and then concentrated in vacuo. The resulting oily residue was taken up in diethyl ether (50 mL), washed with 2N HCl (20 mL), water (20 mL) and brine (20 mL). The organic phase was dried over anhydrous sodium sulfate and evaporated to dryness. The crude compound was purified by column chromatography on silica gel, eluting with 30% ethyl acetate:hexane to give the desired product (11) as a colorless oil, which solidified on further standing at room temperature for 12 h (0.70 g, 78% yield), m.p. 62-64° C.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for one hour
3. concentrationconcentrated in vacuo
4. washwashed with 2N HCl (20 mL), water (20 mL) and brine (20 mL)
5. dry with materialThe organic phase was dried over anhydrous sodium sulfate
6. customevaporated to dryness
7. customThe crude compound was purified by column chromatography on silica gel
8. washeluting with 30% ethyl acetate