反应详情

温度

25 °C

To a solution of 133 (0.5 g, 1.31 mmol) in 1,4-dioxane (5 mL) was added slowly a solution of 1-methylpiperizine (0.13 g, 1.31 mmol) in 1,4-dioxane (5 mL) followed by 2.5 N sodium hydroxide solution (0.5 mL, 1.31 mmol) and water (1.2 mL). The mixture was heated to reflux for 2.5-3 hours with stirring under nitrogen atmosphere and then cooled to 25° C. and diluted with water (10 mL). The mixture was then stirred for 10-15 min., the precipitated solid was filtered off and dried under vacuum to afford the title compound E18 as an off-white solid (0.5 g, 86%). mp 120-122° C.; HPLC: Inertsil ODS 3V (250×4.6 mm) 5 microns 65:35 [0.01 M KH2PO4 (0.1% TFA): CH3CN], 223 nm, Rt 10.23 min, 98.50% purity); MS (CI): m/z 446 (M+H, 100), 375 (25).

1. temperatureThe mixture was heated
2. temperatureto reflux for 2.5-3 hours
3. stirringThe mixture was then stirred for 10-15 min.
4. filtrationthe precipitated solid was filtered off
5. customdried under vacuum