反应详情

A mixture of 12.9 g of 6-chloro-2[(4-methoxyphenyl)amino]-3-nitrobenzoic acid, 25 ml of chlorobenzene and 50 ml of phosphorus oxychloride was stirred and heated to reflux temperature over a period of one hour, and held under reflux for 4.5 hours. The mixture was cooled, filtered, and the filtrate concentrated to a viscous dark residue in vacuo. This residue and the precipitate collected previously were dissolved in 130 ml of acetic acid and cautiously treated with 15 ml of water with stirring. The resulting dark red solid was collected, washed with water, and dried to provide 11.5 g (95%) of the title compound, mp 262°-264° C.

1. temperatureheated
2. temperatureto reflux temperature over a period of one hour
3. temperatureunder reflux for 4.5 hours
4. temperatureThe mixture was cooled
5. filtrationfiltered
6. concentrationthe filtrate concentrated to a viscous dark residue in vacuo
7. customThis residue and the precipitate collected previously
8. dissolutionwere dissolved in 130 ml of acetic acid
9. additioncautiously treated with 15 ml of water
10. stirringwith stirring
11. customThe resulting dark red solid was collected
12. washwashed with water
13. customdried