反应详情

To a solution of potassium tert-butoxide (0.22 g, 1.97 mmol) in THF (7 mL) is added 2,2,2-trifluoroethanol (0.09 mL, 1.28 mmol), and the mixture is stirred at rt for 20 minutes. A solution of 1-(6-chloro-5-methoxypyridin-3-yl)ethanone (0.18 g, 0.99 mmol, Step-2) in THF (8 mL) is added dropwise to the mixture, and the resulting mixture is stirred at rt for 3.5 hours. The reaction mixture is poured into saturated aqueous ammonium chloride solution (20 mL) and extracted with EtOAc (30 mL). The organic layer is dried over sodium sulfate. After filtration, the filtrate is concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (4:1) to give 0.25 g (>99% yield) of the title compound as white solid.

1. stirringthe resulting mixture is stirred at rt for 3.5 hours
2. extractionextracted with EtOAc (30 mL)
3. dry with materialThe organic layer is dried over sodium sulfate
4. filtrationAfter filtration
5. concentrationthe filtrate is concentrated in vacuo
6. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (4:1)