反应详情

To a stirred solution of (3-ethoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)methanamine (2.75 g, 9.54 mmol) in acetonitrile (50 mL) was added 2-chloro-5-iodo-3-nitropyridine (2.85 g, 10.01 mmol) and N,N-diisopropylethylamine (1.85 g, 14.31 mmol). The resulting yellow mixture was heated to reflux. After 3 h, the red-brown solution was allowed to cool to room temperature, resulting in the formation of a precipitate. The solids were isolated by filtration and washed with water (200 mL). The moist solids were dissolved in dichloromethane (100 mL), and a small amount of water separated and was removed. The solution was dried over magnesium sulfate, filtered, and concentrated to provide 4.34 g (85%) of N-(3-ethoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-5-iodo-3-nitropyridin-2-amine as an orange solid.

1. temperatureThe resulting yellow mixture was heated to reflux
2. customresulting in the formation of a precipitate
3. customThe solids were isolated by filtration
4. washwashed with water (200 mL)
5. dissolutionThe moist solids were dissolved in dichloromethane (100 mL)
6. customa small amount of water separated
7. customwas removed
8. dry with materialThe solution was dried over magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated