反应详情

温度

70 °C

A suspension of Na2SO3 (3.26 g, 25.9 mmol) in EtOH (32 ml) and water (40 ml) was added to a solution of 5-chloro-2-fluoro nitrobenzene (2.0 g, 11.4 mmol) in EtOH (24 ml) and the mixture was heated at 70° C. for 16 h. After cooling, the mixture was acidified to pH=2 with conc. HCl (2 ml) and the solvent was removed in vacuo. The residue was diluted with brine solution (12 ml) and the mixture was heated under reflux for 2 h. The solution was cooled in ice bath and the resulting precipitate was collected by filtration to give the title compound (1.54 g, 57%) which was used in the next step without further purification.

1. temperatureAfter cooling
2. customthe solvent was removed in vacuo
3. additionThe residue was diluted with brine solution (12 ml)
4. temperaturethe mixture was heated
5. temperatureunder reflux for 2 h
6. temperatureThe solution was cooled in ice bath
7. filtrationthe resulting precipitate was collected by filtration