反应详情

温度

110 °C

In DMF (50 ml) was dissolved methyl 5-nitrosalicylate (1.97 g, 10.0 mmol), and to the mixture were added ethyl 4-bromobutyrate (1.57 ml, 11.0 mmol) and potassium carbonate (2.76 g, 20.0 mmol). The mixture was stirred at 110° C. for 5 hours, and the mixture was concentrated under reduced pressure. To the residue was added ethyl acetate, and the mixture was washed with water and 10% potassium carbonate solution. The organic layer was dried with anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified with column chromatography (silica gel 30 g, ethyl acetate/hexane=1/5→1/3), and the desired fraction was concentrated under reduced pressure to give ethyl 4-(2-methoxycarbonyl-4-nitrophenoxy)butyrate (2.51 g, 8.06 mmol, 81%).

1. concentrationthe mixture was concentrated under reduced pressure
2. additionTo the residue was added ethyl acetate
3. washthe mixture was washed with water and 10% potassium carbonate solution
4. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified with column chromatography (silica gel 30 g, ethyl acetate/hexane=1/5→1/3)
7. concentrationthe desired fraction was concentrated under reduced pressure