反应详情

温度

25 °C

A mixture of isopropanol (2 mL) and sodium hydroxide (95 mg, 2.27 mmol) in benzene (10 mL) was heated to reflux for 2 hours with stirring under nitrogen atmosphere and then cooled to 25° C. followed by the addition of compound 133 (0.3 g, 0.78 mmol) at same temperature. The mixture was heated to reflux for 6 hours, concentrated under vacuum and diluted with water (10 mL). The precipitated solid was filtered off and purified by column chromatography (1–2% MeOH—CHCl3) to afford the title compound E21 as an off-white solid (0.30 g, 94%). mp 136–138° C.; HPLC: Inertsil ODS 3V (250×4.6 mm) 5 microns [solvent A=0.01 M KH2PO4 (pH 7.0); solvent B═CH3CN], Gradient elution program: T/% B=0/60, 10/60, 25/80, 40/80, 45/60, 50/60; 268 nm, Rt 30.06 min, 98.78% purity; MS (CI): m/z 406 (M+H, 100).

1. temperaturewas heated
2. temperatureto reflux for 2 hours
3. temperatureThe mixture was heated
4. temperatureto reflux for 6 hours
5. concentrationconcentrated under vacuum
6. additiondiluted with water (10 mL)
7. filtrationThe precipitated solid was filtered off
8. custompurified by column chromatography (1–2% MeOH—CHCl3)