反应详情

温度

80 °C

To a stirred solution of 4-hydroxymethylbenzoic acid (3.33 g, 21.9 mmol) in DMF (100 mL), was added potassium carbonate (5.67 g, 41.04 mmol) followed by 2-(3-bromopropyl)-1,3-dioxolane (3.0 g, 19.9 mmol). The resulting mixture was heated at 80° C. for 16 hours. The reaction mixture was diluted with ethyl acetate and washed sequentially with water and twice with brine. The organic phase was dried with anhydrous magnesium sulfate, and filtered, and the filtrate evaporated at reduced pressure. The crude material was purified by silica gel chromatography eluting with 100% iso-hexane to 100% ethyl acetate in iso-hexane to afford the title compound as a colourless oil (2.55 g, 48%).

1. washwashed sequentially with water and twice with brine
2. dry with materialThe organic phase was dried with anhydrous magnesium sulfate
3. filtrationfiltered
4. customthe filtrate evaporated at reduced pressure
5. customThe crude material was purified by silica gel chromatography
6. washeluting with 100% iso-hexane to 100% ethyl acetate in iso-hexane