反应详情

温度

80 °C

To a solution of methyl 5-(4-(4-cyanophenyl)piperidine-1-carbonyl)-2-cyclobutyl-4-ethylbenzoate (compound 215.5, 2.15 g, 4.99 mmol, 1.00 equiv) in methanol (20 mL), was added hydrazine hydrate (80%, 15 mL) batchwise. The reaction was stirred at 80° C. overnight. After cooling to ambient temperature, the mixture was concentrated under reduced pressure. The residue was extracted with dichloromethane (2×100 mL). The combined organic layers were dried over anhydrous magnesium sulfate, and concentrated in vacuo. The residue was purified by silica gel chromatography with dichloromethane/methanol (100:1) to furnish 1.13 g (53%) of the desired product as a pinkish solid.

1. temperatureAfter cooling to ambient temperature
2. concentrationthe mixture was concentrated under reduced pressure
3. extractionThe residue was extracted with dichloromethane (2×100 mL)
4. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica gel chromatography with dichloromethane/methanol (100:1)