反应详情

温度

90 °C

Copper(II) chloride (anhydrous; 2.02 g, 15.05 mmol) was added to a solution of benzyl 4-(6-methyl-3-oxo-2,3,4,5-tetrahydropyridazine-4-yl)piperidine-1-carboxylate (2.48 g, 7.53 mmol) in acetonitrile (26 mL). The reaction mixture was heated at 90° C. After 18 h, the mixture was cooled to ambient temperature and concentrated. The residue was diluted with dichloromethane and 1 N HCl. 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) to give the title compound (1.45 g). MS 328.2 (M+1).

1. temperaturethe mixture was cooled to ambient temperature
2. concentrationconcentrated
3. additionThe residue was diluted with dichloromethane and 1 N HCl
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)