反应详情

温度

55 °C

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). Stir the mixture at 55° C. for 16 hours then cool it to ambient temperature. Pour the mixture onto ice chips and stir for 1 hour. Remove the resulting yellow precipitate by vacuum filtration. Dry the precipitate under vacuum then recrystallize it in ethanol to give 5.15 g (54%) of fine, amber colored needles: mp 162–164°; mass spectrum (ion spray): m/z=254.0 (M+1).

1. temperaturethen cool it to ambient temperature
2. additionPour the mixture onto ice chips
3. stirringstir for 1 hour
4. customRemove the resulting yellow precipitate
5. filtrationby vacuum filtration
6. customDry the precipitate under vacuum
7. customthen recrystallize it in ethanol
8. customto give 5.15 g (54%) of fine, amber colored needles