反应详情

温度

0 °C

To a stirred solution of (3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)methanamine (9.11 g, 33.21 mmol) in acetonitrile (150 mL) was added 2-chloro-5-iodo-3-nitropyridine (9.90 g, 34.81 mmol) and N,N-diisopropylethylamine (6.44 g, 49.81 mmol). The yellow solution was heated to reflux and stirred. After 3 h, the red-brown mixture was cooled to 0° C. resulting in the formation of a precipitate. The precipitate was isolated by filtration and washed with acetonitrile (50 mL) and water (200 mL). The moist solids were dissolved in dichloromethane, and a small amount of water separated and was removed. The organic phase was dried over magnesium sulfate, filtered, and concentrated to provide 14.67 g (85%) of 5-iodo-N-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-3-nitropyridin-2-amine as a yellow-brown solid.

1. temperatureThe yellow solution was heated
2. temperatureto reflux
3. customresulting in the formation of a precipitate
4. customThe precipitate was isolated by filtration
5. washwashed with acetonitrile (50 mL) and water (200 mL)
6. dissolutionThe moist solids were dissolved in dichloromethane
7. customa small amount of water separated
8. customwas removed
9. dry with materialThe organic phase was dried over magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated