反应详情

A solution of 1-tert-butyl 4-methyl 4-(2-oxoethyl)piperidine-1,4-dicarboxylate (822 mg, 2.88 mmol), copper(II) sulfate (1.38 g, 8.64 mmol) and 2-methyl-2-propanesulfinamide (354 mg, 3.17 mmol) in dichloroethane (15 mL) was heated at 65° C. for 24 h. The reaction was cooled, filtered and concentrated. The residue was partitioned between saturated aqueous NaHCO3 and dichloromethane, separated, the organic layer dried over MgSO4, and concentrated. The crude product was purified by silica gel chromatography, eluting with a gradient of 0 to 7% methanol:dichloromethane to give the title compound (0.9 g). MS: m/z=389.2 (M+1).

1. temperatureThe reaction was cooled
2. filtrationfiltered
3. concentrationconcentrated
4. customThe residue was partitioned between saturated aqueous NaHCO3 and dichloromethane
5. customseparated
6. dry with materialthe organic layer dried over MgSO4
7. concentrationconcentrated
8. customThe crude product was purified by silica gel chromatography
9. washeluting with a gradient of 0 to 7% methanol