反应详情

温度

70 °C

A mixture of methyl 4-hydroxybenzoate (1.52 g, 10 mmol), 1,3-dibromo-propane (20.3 mL, 200 mmol) and potassium carbonate (4.2 g, 30 mmol) in 100 mL of dry CH3CN was heated at 70° C. for 5.0 hr. After cooling to room temperature, the reaction mixture was filtered through a pad of Celite and rinsed with CH3CN. The combined filtrates were concentrated in vacuo and purified by ISCO (Hexane-ethyl acetate: 80:20 to 0:100) on silica gel to afford 107A (2.44 g, 89%) as an oil.

1. temperatureAfter cooling to room temperature
2. filtrationthe reaction mixture was filtered through a pad of Celite
3. washrinsed with CH3CN
4. concentrationThe combined filtrates were concentrated in vacuo
5. custompurified by ISCO (Hexane-ethyl acetate: 80:20 to 0:100) on silica gel