反应详情

温度

60 °C

A suspension of 3-fluoro-4-hydroxybenzonitrile (20 g, 0.1459 mol; see step (iv) above), anhydrous K2CO3 (40.33 g, 0.2918 mol) and 1,2-dibromoethane (76.8 mL, 0.8754 mol) in dry DMF (150 mL) was stirred at 60° C. for 5 days under a nitrogen atmosphere. The reaction mixture was filtered through Celite® and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography over silica gel, using 2% ethyl acetate in petroleum ether as eluent, to yield 21.6 g of the sub-title compound as a solid.

1. filtrationThe reaction mixture was filtered through Celite®
2. customthe solvent was evaporated under reduced pressure
3. customThe residue was purified by column chromatography over silica gel