反应详情

To a stirred solution of (3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)methanamine (5.00 g, 18.23 mmol) in acetonitrile (75 mL) was added 1-fluoro-4-iodo-2-nitrobenzene (4.55 g, 17.04 mmol) and diisopropylethylamine (3.30 g, 25.56 mmol). The yellow solution was heated to reflux and stirred. After 4 h, the orange-brown mixture was allowed to cool to room temperature and was diluted with water (150 mL). The resulting bright orange precipitate was isolated by filtration and washed with water. 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 7.10 g (80%) of 4-iodo-N-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-2-nitroaniline as a bright orange solid.

1. temperatureThe yellow solution was heated
2. temperatureto reflux
3. customThe resulting bright orange precipitate was isolated by filtration
4. washwashed with water
5. dissolutionThe moist solids were dissolved in dichloromethane
6. customa small amount of water separated
7. customwas removed
8. dry with materialThe organic phase was dried over magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated