反应详情

A mixture of 3,4,5,6-tetrahydrophthalic anhydride (22.8 g, 150 mmol), 2-fluoro-5-nitroaniline (23.4 g, 150 mmol) in glacial acetic acid is heated at reflux for 23 hours, cooled and poured into a water/toluene mixture. The organic phase is separated, washed sequentially with water and saturated sodium hydrogen carbonate solution, dried and concentrated in vacuo to obtain a yellow solid. Recrystallization of the solid from ethanol gives the title compound as off-white plates (26.6 g, mp 154°-156° C.) which are identified by 1H and 13C NMR spectral analyses.

1. temperatureis heated
2. temperatureat reflux for 23 hours
3. temperaturecooled
4. customThe organic phase is separated
5. washwashed sequentially with water and saturated sodium hydrogen carbonate solution
6. customdried
7. concentrationconcentrated in vacuo
8. customto obtain a yellow solid
9. customRecrystallization of the solid from ethanol