反应详情

Combine 5-methyl-2-(2-nitro-phenylamino)-benzonitrile (4.03 g, 15.91 mmol), tin(II) chloride dihydrate (10.77 g, 47.74 mmol), 5N HCl (65 ml), and ethanol (40.0 ml). Stir the mixture at reflux for 7 hours then cool it to ambient temperature and chill it in the refrigerator overnight. Remove the resulting precipitate by vacuum filtration. Place the precipitate in ethanol (100.0 ml) and 5N HCl (20.0 ml) and heat at reflux for 19 hours. Cool the reaction mixture to ambient temperature then chill it in the refrigerator. Filter off the resulting precipitate by vacuum filtration and dry it in a vacuum oven to give 2.59 g (63%) of an orange solid: mass spectrum (ion spray): m/z=224.0 (M+1).

1. temperatureat reflux for 7 hours
2. temperaturechill it in the refrigerator overnight
3. customRemove the resulting precipitate
4. filtrationby vacuum filtration
5. temperature5N HCl (20.0 ml) and heat
6. temperatureat reflux for 19 hours
7. temperatureCool the reaction mixture to ambient temperature
8. temperaturethen chill it in the refrigerator
9. filtrationFilter off the resulting precipitate
10. filtrationby vacuum filtration
11. customdry it in a vacuum oven