反应详情

温度

140 °C

A stirring suspension of benzyl 4-(methylsulfonyloxy)piperidine-1-carboxylate (1.97 g, 6.30 mmol), 4-hydroxypyridin-2(1H)-one (0.50 g, 4.5 mmol, Aldrich), potassium carbonate (1.43 g, 10.6 mmol, EMD) and DMF (25 mL) was heated at 140° C. for 2.5 h and then cooled to room temperature. The resulting mixture was diluted with H2O and extracted with EtOAc (2×). The organic layers were combined and washed with brine, dried over Na2SO4 and concentrated in vacuo to a light yellow oil. The oil was purified by flash chromatography (SiO2, 0 to 10% MeOH in CH2Cl2) to yield 550 mg of desired product as a white solid. MS (ESI) 329 (M+H).

1. temperaturecooled to room temperature
2. extractionextracted with EtOAc (2×)
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo to a light yellow oil
6. customThe oil was purified by flash chromatography (SiO2, 0 to 10% MeOH in CH2Cl2)