反应详情

4-(3-Fluoro-4-{[1-(4-fluorophenylcarbamoyl)cyclopropanecarbonyl]amino}phenoxy)pyridine-2-carboxamide (101 mg) was dissolved in N,N-dimethylformamide (1.0 ml) under a nitrogen atmosphere, and water (0.01 ml), [bis(trifluoroacetoxy)iodo]benzene (109 mg) and pyridine (0.0541 ml) were added at room temperature in this order, followed by stirring overnight. Water (0.01 ml), [bis(trifluoroacetoxy)iodo]benzene (109 mg) and pyridine (0.0541 ml) were added at room temperature in this order, followed by further stirring for 24 hr. The reaction mixture was partitioned between ethyl acetate and a 1N aqueous solution of sodium hydroxide. The organic layer was separated, washed with brine, and dried over anhydrous sodium sulfate. The solvent was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate). Fractions containing the target compound were concentrated under reduced pressure, and the residue was dried under reduced pressure to provide the titled compound as white foam (62.2 mg, 66%).

1. stirringby further stirring for 24 hr
2. customThe reaction mixture was partitioned between ethyl acetate
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationThe solvent was concentrated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate)
8. additionFractions containing the target compound
9. concentrationwere concentrated under reduced pressure
10. customthe residue was dried under reduced pressure