反应详情

温度

0 °C

2-Chloro-6-fluorobenzoyl chloride (13.6 g, 71.6 mmol) was added dropwise, over 10 minutes, to a solution of 3,5-difluoro-pyridin-4-ylamine (7.7 g, 59.3 mmol) in pyridine (100 mL) at 0° C. under argon and the reaction mixture was stirred at 0° C. for 3 hours. The volatiles were removed under reduced pressure and the resultant residue was treated with 1N HCl (100 mL). The resultant suspension was stirred at room temperature for 2 hours and then the solid was collected by filtration, washing with water. A mixture of 2-chloro-N-(3,5-difluoropyridin-4-yl)-6-fluorobenzamide, LCMS (Method E): RT=2.83 min, m/z: 287 [M+H+], and of 2-chloro-N-(2-chloro-6-fluorobenzoyl)-N-(3,5-difluoropyridin-4-yl)-6-fluorobenzamide LCMS (Method E): RT=3.96 min, m/z: 443 [M+H+], (23 g) was obtained which was used in the following step without further purification.

1. customThe volatiles were removed under reduced pressure
2. additionthe resultant residue was treated with 1N HCl (100 mL)
3. stirringThe resultant suspension was stirred at room temperature for 2 hours
4. filtrationthe solid was collected by filtration
5. washwashing with water
6. additionA mixture of 2-chloro-N-(3,5-difluoropyridin-4-yl)-6-fluorobenzamide, LCMS (Method E)