反应详情

温度

80 °C

To a stirred solution of 3-chloropropyl-1,3-dioxolane (0.2 g, 1.35 mmol) in dimethyl formamide (14 mL), was added 4-((3-(azido(phenyl)methyl)phenoxy)-methyl)benzoic acid (Example 51 Step 3) (0.5 g, 1.39 mmol) and potassium carbonate (0.38 g, 2.78 mmol). The reaction was allowed to stir at 80° C. for 16 hours. The reaction mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate (×3). The organic extracts were washed with brine, dried (sodium sulphate), filtered, and concentrated under reduced pressure. The crude material was purified by silica gel chromatography eluting with 0-100% ethyl acetate in iso-hexane to afford the title compound (0.63 g, 96%).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionextracted with ethyl acetate (×3)
3. washThe organic extracts were washed with brine
4. dry with materialdried (sodium sulphate)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified by silica gel chromatography
8. washeluting with 0-100% ethyl acetate in iso-hexane