反应详情

温度

50 °C

To a solution of 2-chloro-6-methoxy-3-nitropyridine (3 g, 15.91 mmol) in tetrahydrofuran (20 mL) was added methyl-3-amino-2-methylpropanoate (2.05 g, 17.50 mmol) and potassium carbonate (4.40 g, 31.82 mmol). The mixture was stirred at 50° C. for 12 hours. The reaction mixture was concentrated in vacuo and washed with water (20 mL), extracted with acetic ester (20 mL×3). The combined organic phase was dried by anhydrous sodium sulphate, and then filtered. The filtrate was concentrated and purified by column chromatograph silica gel (elute: dichloromethane/Methanol: 100:1→80:1) to give methyl-3-((6-methoxy-3-nitropyridin-2-yl)amino)-2-methylpropanoate (4.2 g, 97%) as a yellow oil.

1. concentrationThe reaction mixture was concentrated in vacuo
2. washwashed with water (20 mL)
3. extractionextracted with acetic ester (20 mL×3)
4. dry with materialThe combined organic phase was dried by anhydrous sodium sulphate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated
7. custompurified by column chromatograph silica gel (elute: dichloromethane/Methanol: 100:1→80:1)