反应详情

温度

100 °C

To an ice cooled suspension of 3-(3-bromo-5-chlorophenoxy)-4-methylpyridin-2-amine (11-4; 600 mg, 1.913 mmol) in 5% aqueous H2SO4 (10 mL) was added a solution of sodium nitrite (198 mg, 2.87 mmol) in water (1 mL) and stirred over ice bath for 30 minutes. After this time, this suspension was added to a solution of 5% aqueous H2SO4 (10 mL) heated to 100° C. and maintained at 100° C. for 1.5 hours. After this time, the mixture was cooled to 0° C. and treated with additional sodium nitrite (60 mg, 0.86 mmol) and then heated to 100° C. for 20 minutes. After this time, the mixture was cooled to 25° C., filtered the resulting solid and washed with water (10 mL) and dried under high vacuum to give the title compound.

1. temperaturemaintained at 100° C. for 1.5 hours
2. temperatureAfter this time, the mixture was cooled to 0° C.
3. temperatureheated to 100° C. for 20 minutes
4. temperatureAfter this time, the mixture was cooled to 25° C.
5. filtrationfiltered the resulting solid
6. washwashed with water (10 mL)
7. customdried under high vacuum