反应详情

m-CPBA (75% in H2O, 89.6 g, 390 mmol) was added portion wise to a stirred solution of N-(5-methylpyridin-2-yl)acetamide (45.0 g, 300 mmol) in DCM (2.7 L) at rt, and the mixture stirred at rt for 4 h. 5% aqueous Na2SO3 (200 mL) was added slowly, the phases were separated and the organic layer washed with saturated NaHCO3, brine (100 mL), dried (MgSO4) and filtered. After concentration in vacuo purification by gradient column chromatography eluting with 2-5% MeOH in DCM yielded the title compound (37.5 g, 243 mmol) as a pale yellow solid.

1. customthe phases were separated
2. washthe organic layer washed with saturated NaHCO3, brine (100 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationAfter concentration
6. customin vacuo purification by gradient column chromatography
7. washeluting with 2-5% MeOH in DCM