反应详情

To a solution of 5-[(2,5-difluorophenyl)[(4-fluorophenyl)sulfonyl]methyl]-N-(1-hydroxymethyl)-4-methylpyridine-2-carboxamide (200 mg, 0.44 mmol) obtained in Example 85 in pyridine (2 ml), acetic anhydride (2 ml) was added, and the mixture was stirred for 3 hours at room temperature. The reaction mixture was concentrated under reduced pressure, and then the residue was dissolved in ethyl acetate, and was washed with water. The solution was dried over anhydrous sodium sulfate and filtered, then the filtrate was concentrated under reduced pressure, and the obtained residue was subjected to silica gel column chromatography. The fraction obtained from an elution with hexane:ethyl acetate=10:3 was concentrated under reduced pressure, washed with diethyl ether, and was collected by filtration, to obtain the title compound (86 mg, 0.17 mmol, 39%) as a white solid.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutionthe residue was dissolved in ethyl acetate
3. washwas washed with water
4. dry with materialThe solution was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe fraction obtained from an elution with hexane
8. concentrationethyl acetate=10:3 was concentrated under reduced pressure
9. washwashed with diethyl ether
10. filtrationwas collected by filtration