反应详情

To a suspension of 2-nitro-5-chloroaniline (5.00 g) in conc. hydrochloric acid (30 ml) under cooling with ice, was added a solution of sodium nitrite (2.10 g) in water (10 ml) dropwise and the mixture was stirred for 30 minutes. Under cooling with ice, to this solution was added a solution of potassium iodide (5.30 g) in water (20 ml) dropwise and the mixture was stirred for 1 hour at room temperature. The solid that appeared was collected by filtration and was dissolved in ethyl acetate and was dried and concentrated to give a crude product of the title compound. It was purified by recrystallization from ethyl acetate-hexane to give the title compound having the following physical data (5.14 g, yellow powder).

1. temperatureunder cooling with ice
2. temperatureUnder cooling with ice, to this solution
3. stirringthe mixture was stirred for 1 hour at room temperature
4. filtrationThe solid that appeared was collected by filtration
5. dissolutionwas dissolved in ethyl acetate
6. customwas dried
7. concentrationconcentrated