反应详情

To a solution of Example 3D (4.6 g, 11 mmol) in tetrahydrofuran was added conc. HCl (6.9 mL). The reaction mixture was refluxed overnight and then cooled to room temperature. 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 using an Analogix® IT280™ (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 overnight
2. extractionextracted with ethyl acetate (3×50 mL)
3. dry with materialThe combined organic extracts were dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by column chromatography