反应详情

温度

-78 °C

To a solution of 6,7-dimethoxy-4-phenylsulfanyl-quinoline (Step a, 1.0 g, 3.4 mmol) in CH2Cl2 (30 mL) at −78° C., 3-chloroperoxybenzoic acid (0.64 g, 3.7 mmol) was added in CH2Cl2 dropwise slowly. The reaction was stirred at −78° C. for 2 h. The solution was poured into saturated NaHCO3 and extracted with CH2Cl2 3×. The combined organic layer was washed with saturated NaHCO3, water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude material was purified by silica gel column chromatography with (70-100% EtOAc/Hexane) to give the titled compound as a white solid. MS (ESI, pos. ion) m/z: 314.4 (M+1).

1. extractionextracted with CH2Cl2 3×
2. washThe combined organic layer was washed with saturated NaHCO3, water and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by silica gel column chromatography with (70-100% EtOAc/Hexane)