反应详情

温度

100 °C

To a solution of 2-methyl-5-(methyloxy)phenol (Intermediate 12, 2 g) and 2-chloro-5-nitropyridine (2.1 g, 13.2 mmol) in DMF (50 mL) was added potassium carbonate (2.76 g, 20 mmol) and the reaction mixture was stirred at 100° C. overnight. The mixture was evaporated under vacuum and water (100 mL) was added. It was extracted with ethyl acetate (3 times 100 mL) and the combined organic layers were dried over sodium sulphate and evaporated to afford a brown oil, which was purified by column chromatography on silica gel (mobile phase: EtOAc/PE=1/50-1/20) to give the title compound (1.5 g).

1. customThe mixture was evaporated under vacuum and water (100 mL)
2. additionwas added
3. extractionIt was extracted with ethyl acetate (3 times 100 mL)
4. dry with materialthe combined organic layers were dried over sodium sulphate
5. customevaporated
6. customto afford a brown oil, which
7. customwas purified by column chromatography on silica gel (mobile phase: EtOAc/PE=1/50-1/20)