反应详情

温度

60 °C

To a solution of 2-methyl-3-(methyloxy)phenol (Intermediate 59, 1.3 g) in DMF (50 mL) was added sodium hydride (60% in mineral oil, 480 mg, 0.012 molat 0° C. and the mixture was stirred for 30 minutes. 2-Chloro-5-nitropyridine (1.9 g, 0.012 mol, Aldrich) was added and the mixture was heated at 60° C. for 3 hours. The mixture was poured into H2O (100 mL) and extracted with ethyl acetate (4 times 100 mL). The combined ethyl acetate phases were dried over sodium sulphate and concentrated under vacuum to give a residue which was purified by column chromatography on silica gel (PE:EtOAc=10:1) to afford the title compound (2.3 g) as a liquid.

1. extractionextracted with ethyl acetate (4 times 100 mL)
2. dry with materialThe combined ethyl acetate phases were dried over sodium sulphate
3. concentrationconcentrated under vacuum
4. customto give a residue which
5. customwas purified by column chromatography on silica gel (PE:EtOAc=10:1)