反应详情

温度

80 °C

Phosphorus oxychloride (1.00 mL) was added to DMF (5.0 mL), and stirred at 80° C. for 30 minutes. A solution prepared by dissolving [3-(piperidin-1-ylsulfonyl)phenyl]methanol (2.00 g) obtained in Reference Example 21 in DMF (5.0 mL) was added to it, and stirred at 80° C. for 30 minutes. At 0° C., aqueous saturated sodium carbonate solution was added thereto, and extracted with ethyl acetate. The organic layer was washed with water and saturated brine in that order, and dried with sodium sulfate. The drying agent was removed through filtration, and the solvent was evaporated off under reduced pressure. The residue was purified through silica gel column chromatography (ethyl acetate/hexane=from 0% to 50%, gradient) to give the entitled compound (1.26 g, 59%) as a colorless solid.

1. customA solution prepared
2. additionwas added to it
3. stirringstirred at 80° C. for 30 minutes
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with water and saturated brine in that order
6. dry with materialdried with sodium sulfate
7. customThe drying agent was removed through filtration
8. customthe solvent was evaporated off under reduced pressure
9. customThe residue was purified through silica gel column chromatography (ethyl acetate/hexane=from 0% to 50%, gradient)