反应详情

To a mixture of 6-chloro-4-methylpyridin-3-ol (2.00 g, 13.9 mmol) and cesium carbonate (6.81 g, 20.9 mmol) in DMF (40 mL) is added dropwise 2,2,2-trifluoroethyl trifluoromethanesulfonate (3.56 g, 15.3 mmol) at 0° C. After stirring at rt for 1 hour, the mixture is poured onto water (300 mL). The aqueous layer is extracted with EtOAc (300 mL). The separated organic layer is washed with water (200 mL), dried over sodium sulfate, and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (9:1) to give 3.00 g (95% yield) of the title compound as white solid.

1. additionthe mixture is poured onto water (300 mL)
2. extractionThe aqueous layer is extracted with EtOAc (300 mL)
3. washThe separated organic layer is washed with water (200 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (9:1)