反应详情

Water (3 mL) and Oxone(R) (853 mg) were sequentially added to a solution of 3-chloro-6-{(E)-2-cyclopentyl-1-[4-(methylsulfanyl)phenyl]ethenyl}pyridin-2(1H)-one obtained in Example 1-1 (160 mg) in THF-methanol (1:1, 6 mL), and the mixture was stirred at room temperature for one hour. The reaction solution was poured into water, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform:hexane=10:0→9:1). The resulting crude product was recrystallized from a chloroform:ethyl acetate:hexane (1:1:1, 6 mL) solution to give the title compound as a colorless powder (130 mg, 74%).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customThe solvent was then evaporated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (chloroform:hexane=10:0→9:1)
7. customThe resulting crude product was recrystallized from a chloroform:ethyl acetate:hexane (1:1:1, 6 mL) solution