反应详情

To a methylene chloride (2 ml) solution of the [5-chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amine (104 mg, 0.242 mmol) obtained in Example 196 and pyridine (74 μl, 0.533 mmol) was added (4-pyridylmethyl)sulfonyl chloride triflate (91 mg, 0.266 mmol). The resulting mixture was stirred at room temperature for 17 hours. To the reaction mixture were added pyridine (74 μl, 0.533 mmol) and (4-pyridylmethyl)sulfonyl chloride triflate (91 mg, 0.266 mmol). The resulting mixture was stirred at room temperature for 19 hours. The reaction mixture was diluted with ethyl acetate. The diluted solution was washed with water 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 (=1:40) eluate was concentrated under reduced pressure to give the title compound (66 mg, 0.113 mmol, 47%) as a white solid.

1. stirringThe resulting mixture was stirred at room temperature for 19 hours
2. washThe diluted solution was washed with water and brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure
6. customThe residue thus obtained
7. concentrationmethylene chloride (=1:40) eluate was concentrated under reduced pressure