反应详情

温度

25 °C

A solution of 2,2,2-trichloroethylchloroformate (Troc—Cl) (1.66 mL, 12.1 mmol) in dry dichloromethane (25 mL) was added drop wise to a solution of 4-nitroanthranilic acid 144 (2 g, 11 mmol) and pyridine (1.78 mL, 22 mmol) in dichloromethane (25 ml) at 0° C. The solution was allowed to stir at 25° C. for 5 hours. The reaction mixture was washed with dilute HCl (1N, 2×50 mL), water (1×50 mL), brine (1×2 5 mL) and dried over MgSO4. Removal of excess solvent by rotary evaporation under reduced pressure afforded the crude product which was used in the subsequent reaction without further purification.

1. washThe reaction mixture was washed with dilute HCl (1N, 2×50 mL), water (1×50 mL), brine (1×2 5 mL)
2. dry with materialdried over MgSO4
3. customRemoval of excess solvent
4. customby rotary evaporation under reduced pressure