反应详情

温度

90 °C

Copper(II) chloride (anhydrous; 101 mg, 0.75 mmol) was added to a solution of benzyl 4-(6-cyclopropyl-3-oxo-2,3,4,5-tetrahydropyridazine-4-yl)piperidine-1-carboxylate (134 mg, 0.38 mmol) in acetonitrile (16 mL). The reaction mixture was heated to 90° C. After 18 h, the mixture was cooled to ambient temperature and concentrated. Dichloromethane was added to the concentrated mixture, followed by hydrochloric acid (1 N in water). The mixture was extracted with dichloromethane (3×) and the combined organic extracts were dried over magnesium sulfate and concentrated. Purification by silica gel chromatography (100% dichloromethane→90% dichloromethane/methanol) gave the title compound (54 mg). MS 354.1 (M+1).

1. temperaturethe mixture was cooled to ambient temperature
2. concentrationconcentrated
3. additionDichloromethane was added to the concentrated mixture
4. extractionThe mixture was extracted with dichloromethane (3×)
5. dry with materialthe combined organic extracts were dried over magnesium sulfate
6. concentrationconcentrated
7. customPurification by silica gel chromatography (100% dichloromethane→90% dichloromethane/methanol)