反应详情

To 2,4-difluoro-phenylamine (1, 7.0 mL, 70.0 mmol) in 100 mL of dichloromethane, pyridine (11 mL, 140.0 mmol) and benzyl chloroformate (2, 11.9 mL, 83.4 mmol) were added. The reaction mixture was stirred at room temperature for 1.5 hours. The reaction mixture was concentrated under vacuum and the residue was partitioned between ethyl acetate and potassium bisulfate solution. The organic layer was dried with magnesium sulfate, filtered and the filtrate concentrated under vacuum and crystallized from hexanes to give the desired compound (3, 15.6 g, 85%).

1. concentrationThe reaction mixture was concentrated under vacuum
2. customthe residue was partitioned between ethyl acetate and potassium bisulfate solution
3. dry with materialThe organic layer was dried with magnesium sulfate
4. filtrationfiltered
5. concentrationthe filtrate concentrated under vacuum
6. customcrystallized from hexanes