反应详情

3.31 g 3-amino-2-chloropyridine (25.8 mmol) and 20 mL pyridine were mixed in an ice bath. 5.0 g 2,3-difluoro-benzoyl chloride (28.4 mmol) was then added. After return to room temperature and reaction for 4 hr, the reaction was quenched by water. After extraction three times by ethyl acetate, an ethyl acetate layer was collected and washed by 1M HCl solution. After drying, filtration, concentration, and purification by silicon-gel column, 6.4 g solid was obtained, with a yield of 93%.

1. customAfter return to room temperature and reaction for 4 hr
2. customthe reaction was quenched by water
3. extractionAfter extraction three times by ethyl acetate
4. customan ethyl acetate layer was collected
5. washwashed by 1M HCl solution
6. customAfter drying
7. filtrationfiltration, concentration, and purification by silicon-gel column