反应详情

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride was added to a pyridine (500 ml) solution of methyl 4-amino-2-fluorobenzoate (18.9 g) and picolinic acid (16.5 g), and stirred at room temperature for 2 hours. The solvent was evaporated away under reduced pressure, ethyl acetate (600 ml) was added to it, and the organic layer was washed with aqueous 0.25 N hydrochloric acid solution, aqueous 0.25 N sodium hydroxide solution and saturated saline water. After dried, this was concentrated under reduced pressure, and solidified from a mixed solvent of hexane/ethyl acetate, and taken out through filtration. After dried under reduced pressure, the entitled compound was obtained as a white solid.

1. customThe solvent was evaporated away under reduced pressure, ethyl acetate (600 ml)
2. additionwas added to it
3. washthe organic layer was washed with aqueous 0.25 N hydrochloric acid solution, aqueous 0.25 N sodium hydroxide solution and saturated saline water
4. customAfter dried
5. concentrationthis was concentrated under reduced pressure
6. filtrationtaken out through filtration
7. customAfter dried under reduced pressure
8. customthe entitled compound was obtained as a white solid