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 then cool it to ambient temperature. Pour the mixture onto ice chips and stir for 1 hour. Remove the resulting precipitate by vacuum filtration. Dry the precipitate under vacuum then purify it on silica gel using dichloromethane/hexanes (75:25) to give 4.45 g (57%) of an orange solid: mp 135–139°; 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 precipitate
5. filtrationby vacuum filtration
6. customDry the precipitate under vacuum
7. customthen purify it on silica gel