反应详情

温度

60 °C

A solution of 3-bromo-4-hydroxybenzonitrile (Intermediate 43; 25.0 g, 126 mmol) in anhydrous acetone (400 ml) was treated with Potassium carbonate (20.8 g, 151 mmol) and dropwise with tert-butyl bromoacetate (24.5 g, 126 mmol). The reaction mixture was heated at 60° C. for 10 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The crude material was purified by column chromatography (silica) eluting with petroleum ether and ethyl acetate (90:10) to afford the title compound as a brown solid.

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate was concentrated under reduced pressure
3. customThe crude material was purified by column chromatography (silica)
4. washeluting with petroleum ether and ethyl acetate (90:10)