反应详情

To a methylene chloride (5 ml) solution of the [5-chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amine (93 mg, 0.217 mmol) obtained in Example 196 and pyridine (21 μl, 0.260 mmol) was added 1-methyl-1H-imidazole-4-sulfonyl chloride (47 mg, 0.260 mmol). The resulting mixture was stirred at room temperature for 18 hours. After pyridine (1 ml) was added to the reaction mixture and the resulting mixture was stirred at room temperature for 7 hours, the reaction mixture was concentrated under reduced pressure. To the residue thus obtained was added ethyl acetate. The resulting mixture was washed sequentially with a saturated aqueous solution of sodium bicarbonate and brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the methanol:methylene chloride (=1:50) eluate was concentrated under reduced pressure to yield a white solid. The resulting white solid was washed with ethanol, and collected by filtration to give the title compound (68 mg, 0.119 mmol, 55%) as a white powder.

1. stirringthe resulting mixture was stirred at room temperature for 7 hours
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. customTo the residue thus obtained
4. washThe resulting mixture was washed sequentially with a saturated aqueous solution of sodium bicarbonate and brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationThe filtrate was concentrated under reduced pressure
8. customThe residue thus obtained
9. concentrationmethylene chloride (=1:50) eluate was concentrated under reduced pressure
10. customto yield a white solid
11. washThe resulting white solid was washed with ethanol
12. filtrationcollected by filtration