反应详情

Into a solution of 3-chloro-4-fluoro-6-nitroaniline (200.3 g) in acetic acid (1.5 litter) was added bromine (339 g) during a period of 80 minutes at 50° C. under stirring and stirred for further 2 hours. The reaction mixture was poured into ice water (3 litter) and the resulting precipitate was collected by filtration, washed with water and added to a mixture of concentrated hydrochloric acid (300 ml) and ethanol (1.2 litter). The mixture was refluxed for 8.5 hrs. After cooling, the precipitate was collected by filtration and washed with water and dried. The title compound thus obtained weighed 235.6 g as yellow needles, mp 146°-147° C.

1. stirringstirred for further 2 hours
2. filtrationwas collected by filtration
3. washwashed with water
4. additionadded to a mixture of concentrated hydrochloric acid (300 ml) and ethanol (1.2 litter)
5. temperatureThe mixture was refluxed for 8.5 hrs
6. temperatureAfter cooling
7. filtrationthe precipitate was collected by filtration
8. washwashed with water
9. customdried