反应详情

KOH (15.7 g, 238 mmol) in water (50 mL), followed by carbon disulfide (14.4 mL, 238 mmol), was added to a solution of 4-chloro-5-iodobenzene-1,2-diamine (50 g, 198 mmol) in EtOH (300 mL). The mixture was heated at reflux for 3 h, cooled and filtered. To the filtrate was added water (300 mL) and then AcOH (25 mL) in water (50 mL). The resulting precipitate was collected, washed with water and a small amount of EtOH, and then dried to afford the desired product as a brown powder, which was used in the next step without further purification.

1. temperatureThe mixture was heated
2. temperatureat reflux for 3 h
3. temperaturecooled
4. filtrationfiltered
5. additionTo the filtrate was added water (300 mL)
6. customThe resulting precipitate was collected
7. washwashed with water
8. dry with materiala small amount of EtOH, and then dried