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) and stir the mixture at reflux. After 7 hours, cool to ambient temperature and chill in the refrigerator overnight. Remove the resulting precipitate by vacuum filtration and 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 and chill 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
2. temperaturechill in the refrigerator overnight
3. customRemove the resulting precipitate
4. filtrationby vacuum filtration and place the precipitate in ethanol (100.0 ml)
5. temperature5N HCl (20.0 ml) and heat
6. temperatureat reflux for 19 hours
7. temperatureCool the reaction mixture to ambient temperature
8. temperaturechill in the refrigerator
9. filtrationFilter off the resulting precipitate
10. filtrationby vacuum filtration
11. customdry it in a vacuum oven