反应详情

温度

55 °C

Combine 1-fluoro-2-nitro-benzene (4.34 g, 30.79 mmol), 2-amino-5-methyl-benzonitrile (4.07 g, 30.79 mmol), lithium hydroxide monohydrate (2.58 g, 61.58 mmol) and DMSO (50.0 ml). Stir the mixture at 55° C. for 22 hours, cool to ambient temperature and pour the mixture onto ice chips and stir. After 1 hour, remove the resulting precipitate by vacuum filtration. Dry the precipitate under vacuum, purify on silica gel using dichloromethane/hexanes (75:25) to give 4.45 g (57%) of an orange solid: mp 135-139° C.; mass spectrum (ion spray): m/z=254.0 (M+1).

1. temperaturecool to ambient temperature
2. additionpour the mixture onto ice chips
3. stirringstir
4. waitAfter 1 hour
5. customremove the resulting precipitate
6. filtrationby vacuum filtration
7. customDry the precipitate under vacuum
8. custompurify on silica gel