反应详情

To a solution of 2-methyl-5-(methyloxy)phenol (Intermediate 12, 1.5 g) and 1-fluoro-4-nitrobenzene (1.4 g, 10.0 mmol) in acetonitrile (100 mL) was added potassium carbonate (2.1 g, 15.2 mmol) and the mixture was stirred at reflux for 5 hours. The resulting mixture was concentrated and partitioned between ethyl acetate (3 times 30 mL) and water (100 mL). The combined ethyl acetate layers were dried over sodium sulphate, filtered and concentrated under vacuum. The crude product thus obtained was purified by column chromatography on silica gel (EtOAc:PE=1:20) to afford the title compound as a solid (2.5 g).

1. temperatureat reflux for 5 hours
2. concentrationThe resulting mixture was concentrated
3. custompartitioned between ethyl acetate (3 times 30 mL) and water (100 mL)
4. dry with materialThe combined ethyl acetate layers were dried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe crude product thus obtained
8. customwas purified by column chromatography on silica gel (EtOAc:PE=1:20)