反应详情

To a solution of 5-[(2,5-difluorophenyl)[(4-fluorophenyl)sulfonyl]methyl]-4-methylpyridine-2-carboxylic acid (105 mg, 0.25 mmol) obtained in Example 12 in methylene chloride (3 ml), dimethylamine hydrochloride (23 mg, 0.28 mmol), 1-hydroxybenzotriazole (37 mg, 0.28 mmol), 4-methylmorpholine (0.061 ml, 0.55 mmol), and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (53 mg, 0.28 mmol) were added at room temperature. After stirring for 3 hours at room temperature, water was added to the reaction mixture, and the mixture was washed with saturated aqueous sodium hydrogencarbonate. The organic layer was dried over anhydrous sodium sulfate and filtered, then the filtrate was concentrated under reduced pressure, and the resulting residue was subjected to flash silica gel chromatography. The fraction obtained from an elusion with hexane:ethyl acetate=3:2 was concentrated under reduced pressure, and the resulting residue was washed with a mixed solvent of ethanol and hexane, and was collected by filtration, to obtain the title compound (77 mg, 0.17 mmol, 69%) as a white solid.

1. washthe mixture was washed with saturated aqueous sodium hydrogencarbonate
2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
3. filtrationfiltered
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe fraction obtained from an elusion with hexane
6. concentrationethyl acetate=3:2 was concentrated under reduced pressure
7. washthe resulting residue was washed with a mixed solvent of ethanol and hexane
8. filtrationwas collected by filtration