反应详情

温度

70 °C

To a solution of N-[(1R)-1-(5-fluoro-2-pyridinyl)ethyl]-3-formyl-5-(5-methyl-2-pyridinyl)benzamide (1.10 g, 3.01 mmol) in dioxane (15 mL) hydroxylamine hydrochloride salt (0.314 g, 4.52 mmol) and pyridine (0.73 mL, 9.04 mmol). The reaction mixture was stirred at 70° C. for 18 h. The mixture was cooled to ambient temperature. Saturated aqueous ammonium chloride and water were added. The mixture was extracted with dichloromethane (3×). The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography (95% dichloromethane/methanol→85% dichloromethane/methanol) gave the title compound (0.91 g). MS 379.1 (M+1).

1. temperatureThe mixture was cooled to ambient temperature
2. extractionThe mixture was extracted with dichloromethane (3×)
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by silica gel chromatography (95% dichloromethane/methanol→85% dichloromethane/methanol)