反应详情

温度

80 °C

To a suspension of compound 10a (0.85 g, 1.8 mmol) in acetic acid (20 mL) was added iron powder (0.50 g, 8.9 mmol). The reaction mixture was stirred at 80° C. for 2 h, and allowed to cool to rt. The reaction mixture was treated with water, and the pH of the solution was adjusted to ca. pH 7 using 3 N NaOH solution. The mixture was extracted with DCM (3×100 mL). The combined organic layers were dried over MgSO4, filtered, and concentrated to obtain compound 10b as a dark red solid. Mass Spectrum (LCMS, ESI pos.): Calcd. for C27H24N6O: 449.2 (M+H). found: 449.1.

1. temperatureto cool to rt
2. extractionThe mixture was extracted with DCM (3×100 mL)
3. dry with materialThe combined organic layers were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated