反应详情

To a stirred solution of Compound 39 (1.0 g) in acetone (30 ml) was added conc. HCl (4 ml) at room temperature. The reaction mixture was stirred at room temperature for 5 h. The solvent was evaporated in vacuo and the residue was extracted with ether. The combined solution was washed with sat. NaHCO3 aq. , and brine, dried(MgSO4) and concentrated in vacuo to give crude product (790 mg) as a yellow solid. The crude product was purified by column chromatography on silica gel with hexane-isopropyl ether(10:1-3:1) to give Compound 40 (275 mg) as a pale yellow solid.

1. customThe solvent was evaporated in vacuo
2. extractionthe residue was extracted with ether
3. washThe combined solution was washed with sat. NaHCO3 aq. , and brine, dried(MgSO4)
4. concentrationconcentrated in vacuo
5. customto give crude product (790 mg) as a yellow solid
6. customThe crude product was purified by column chromatography on silica gel with hexane-isopropyl ether(10:1-3:1)