反应详情

Combine 1-fluoro-2-nitro-benzene (5.34 g, 37.83 mmol), 2-amino-4-methyl-benzonitrile (5.00 g, 37.83 mmol), lithium hydroxide monohydrate (3.17 g, 75.66 mmol) and DMSO (70.0 ml) and stir at 55° C. Afer 16 hours; cool to ambient temperature, pour the mixture onto ice chips and stir. After 1 hour, remove the resulting yellow precipitate by vacuum filtration. Dry the precipitate under vacuum, recrystallize in ethanol to give 5.15 g (54%) of fine, amber colored needles: mp 162-164° C.; mass spectrum (ion spray): m/z 254.0 (M+1).

1. customAfer 16 hours
2. additionpour the mixture onto ice chips
3. customremove the resulting yellow precipitate
4. filtrationby vacuum filtration
5. customDry the precipitate under vacuum
6. customrecrystallize in ethanol
7. customto give 5.15 g (54%) of fine, amber colored needles