反应详情

温度

0 °C

To a solution of concentrated H2SO4 (5 mL) in water (15 mL), 5-chloro-2,4-dimethoxy-phenylamine (3 g, 16 mmol) was added, resulting a deep purple suspension. More water (15 mL) was then added and the mixture was cooled and stirred vigorously at 0° C. in an ice-salt bath. A solution of sodium nitrite (1.2 g, 17.4 mmol) in water (5 mL) was added slowly and a brown solution was obtained. This solution was stirred at this temperature for an hour. After that, a solution of sodium azide (1.2 g, 18.5 mmol) in water (10 mL) was followed and the solution turned grey. This solution was then stirred for an hour. The grey precipitations (1.0 g, 30%) formed were collected, washed with water and dried. Yellow solids formed in the filtrate were also collected, washed and dried. The second crop (1.47 g, 43%) turned to light grey quickly.

1. customresulting a deep purple suspension
2. temperaturethe mixture was cooled
3. customa brown solution was obtained
4. stirringThis solution was stirred at this temperature for an hour
5. stirringThis solution was then stirred for an hour
6. customThe grey precipitations (1.0 g, 30%)
7. customformed
8. customwere collected
9. washwashed with water
10. customdried
11. customYellow solids formed in the filtrate
12. customwere also collected
13. washwashed
14. customdried