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温度

0 °C

To a mixture of 6-chloro-2-hydroxy-4-(tetrahydro-pyran-2-yloxy)benzaldehyde (10.5 g, 40.9 mmol) and pyridine (14.6 mL, 0.20 mol) in DCM (150 mL) cooled at −10˜0° C. was added Tf2O (10.3 mL, 61.2 mmol) dropwise. The reaction mixture was stirred at 0° C. for an additional 2 h and quenched with cold brine (40 mL). The resulting mixture was extracted with EtOAc (2×50 mL). The combined organic layers were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by column chromatography on silica gel (EtOAc: PE=1:200) to give the title compound as a yellow oil (10.5 g. Yield: 66%).

1. temperaturecooled at −10˜0° C.
2. customquenched with cold brine (40 mL)
3. extractionThe resulting mixture was extracted with EtOAc (2×50 mL)
4. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography on silica gel (EtOAc: PE=1:200)