反应详情

To a solution of (4-fluoro-phenyl)-(5-hydroxymethyl-pyridin-3-yl)-methanone (1I) (410 mg, 1.8 mmol) in 25 mL of acetonitrile at 0° C., is added thionyl chloride (0.65 mL, 8.9 mmol) drop wise. After being stirred at room temperature for 2 hours, the reaction mixture is concentrated to remove most of thionyl chloride and acetonitrile. The residue is dissolved in 30 mL of CH2Cl2 and basified by saturated sodium bicarbonate to PH˜8.0. The organic layer is dried over sodium sulfate and concentrated to give (5-chloromethyl-pyridin-3-yl)-(4-fluoro-phenyl)-methanone (1J) (390 mg, yield 87%) as light yellow waxy solid. MS (ESI) m/e 250 (M+H+).

1. concentrationthe reaction mixture is concentrated
2. customto remove most of thionyl chloride and acetonitrile
3. dissolutionThe residue is dissolved in 30 mL of CH2Cl2
4. dry with materialThe organic layer is dried over sodium sulfate
5. concentrationconcentrated