反应详情

To a solution of Example 251D (4.6 g, 11 mmol) in tetrahydrofuran was added concentrated HCl (6.9 mL). The reaction mixture was heated at reflux 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 CH2Cl2) to afford the title compound. MS (ESI+) m/z 185 (M+H)+.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for overnight
3. temperaturecooled
4. extractionextracted with ethyl acetate (3×50 mL)
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by column chromatography (SiO2, 0-10% methanol in CH2Cl2)