反应详情

To a solution of phenyl N-[4-(3-fluoro-4-{[1-(phenylcarbamoyl)cyclopropanecarbonyl]amino}phenoxy)pyridin-2-yl]-N-phenoxycarbonylcarbamate (50.0 mg) in N,N-dimethylformamide (1.0 ml) was added (3S)-(−)-3-dimethylaminopyrrolidine (44 mg), followed by stirring at room temperature for 3.5 hr. The reaction mixture was partitioned between ethyl acetate and 1N sodium hydroxide. The organic layer was washed with brine, and dried over anhydrous sodium sulfate. The solvent was removed, and the residue was purified by silica gel column chromatography (Fuji Silysia NH, ethyl acetate:methanol=98:2). Fractions containing the target compound were concentrated. A solid was precipitated by addition of diethyl ether:hexane=1:2 to the residue. The solvent was removed, and the residue was dried under reduced pressure to provide the titled compound as white powder (36.1 mg, 85%).

1. customThe reaction mixture was partitioned between ethyl acetate and 1N sodium hydroxide
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous sodium sulfate
4. customThe solvent was removed
5. customthe residue was purified by silica gel column chromatography (Fuji Silysia NH, ethyl acetate:methanol=98:2)
6. additionFractions containing the target compound
7. concentrationwere concentrated
8. customA solid was precipitated by addition of diethyl ether
9. customThe solvent was removed
10. customthe residue was dried under reduced pressure