反应详情

Add methanesulfonyl chloride (1.8 mL, 23.5 mmol) to a solution of (5-fluoro-pyridin-2-yl)-methanol (2.5 g, 19.7 mmol) and triethylamine (8.2 mL, 59.0 mmol) in DCM (150 mL) at 0° C. under nitrogen. Stir the mixture for 30 min and concentrate in vacuo. Dilute with water (20 mL) and extract the mixture with EtOAc (3×50 mL). Combine the organic extracts and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc to obtain the desired intermediate (2.2 g, 54%).

1. concentrationconcentrate in vacuo
2. additionDilute with water (20 mL)
3. extractionextract the mixture with EtOAc (3×50 mL)
4. concentrationCombine the organic extracts and concentrate in vacuo
5. customPurify by chromatography on silica gel eluting with hexane/EtOAc