反应详情

To a solution of Example 89D (4.6 g, 11 mmol) in THF (90 mL) was added conc. HCl (6.9 mL). The reaction mixture was refluxed for overnight and then cooled. The mixture was basified with 5N NaOH ((17 mL) and extracted with ethyl acetate (3×50 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The residue was purified by column chromatography (SiO2, 0-10% methanol in dichloromethane) to afford 1.04 g (51%) of the title compound. MS (ESI+) m/z 185 (M+H)+

1. temperatureThe reaction mixture was refluxed for overnight
2. temperaturecooled
3. extractionextracted with ethyl acetate (3×50 mL)
4. dry with materialThe combined organic extracts were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by column chromatography (SiO2, 0-10% methanol in dichloromethane)