反应详情

To 8.0 g (20 mmol) 4-(3-Chloro-4-methoxyphenylmethylamino)-6-cyanoquinoline-3-carboxylic acid ethyl ester was added 100 mL THF, 100 mL MeOH and 100 mL 1M NaOH, and the resulting mixture was stirred well. The solids gradually dissolved as the reaction progressed. After 1 h, the THF and most of the MeOH was evaporated under reduced pressure to leave an aqueous slurry of a white solid. The slurry was acidified to pH 1.5 with HCl, stirred well for 1 h, and then filtered and washed well with water to give 7.5 g (20 mmol, 100% yield) of a white chalky solid. Codistilling twice to dryness with absolute ethanol afforded the title compound: LC/MS: M/Z 368 (M+H) observed, 90+% purity; mp: decomposed 255-260° C. LC 2.93°.

1. dissolutionThe solids gradually dissolved as the reaction
2. customthe THF and most of the MeOH was evaporated under reduced pressure
3. customto leave an aqueous slurry of a white solid
4. stirringstirred well for 1 h
5. filtrationfiltered
6. washwashed well with water
7. customto give 7.5 g (20 mmol, 100% yield) of a white chalky solid