反应详情

温度

80 °C

To a stirred solution of benzyl 3-bromo-5-hydroxybenzoate (2.85 g, 9.22 mmol) in dimethyl formamide (50 mL), was added 2-(8-bromooctyl)-1,3-dioxolane (2.44 g, 9.21 mmol) and potassium carbonate (1.91 g, 13.8 mmol), and the mixture stirred at 80° C. for 16 hours. The reaction mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate (×3). The combined organic extracts were washed with brine, dried (magnesium sulphate), filtered, and concentrated under reduced pressure. The crude material was purified by silica gel chromatography eluting with 0-7% ethyl acetate in iso-hexane to afford the title compound (2.94 g, 65%).

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