反应详情

温度

100 °C

To a suspension of 3-[(2-amino-4-chloropyridin-3-yl)oxy]-5-chlorobenzonitrile (590 mg, 2.106 mmol) in 5% aqueous H2SO4 (20 mL) cooled over an ice bath for 5 minutes was added sodium nitrite (247 mg, 3.58 mmol) and stirred 5 minutes. This mixture was then heated to 100° C. for 5 minutes. The mixture was re-cooled over an ice bath and treated with additional sodium nitrite (124 mg, 1.79 mmol), stirred cold for another 5 minutes and then heated to 100° C. for 5 minutes. The reaction mixture was again cooled over an ice bath and the resulting white solid was filtered and washed with water (4×5 mL). This solid was dried under high vacuum to provide the title compound. LRMS (M+1): 280.7.

1. temperaturecooled over an ice bath for 5 minutes
2. temperatureThe mixture was re-cooled over an ice bath
3. stirringstirred cold for another 5 minutes
4. temperatureheated to 100° C. for 5 minutes
5. temperatureThe reaction mixture was again cooled over an ice bath
6. filtrationthe resulting white solid was filtered
7. washwashed with water (4×5 mL)
8. customThis solid was dried under high vacuum