反应详情

温度

0 °C

TEA (2.28 g, 0.023 mol) was added at once to a solution of 3 g (0.0206 mol) 4-chloro-3-fluoroaniline in 50 ml of DCM and then ethyl 2-chloro-2-oxoacetate (2.81 g, 0.0206 mol) was added dropwise at 0° C. Reaction mixture was stirred at 0° C. for 1 h and then continued at room temperature (RT) for 6 h. The mixture was washed with 25% aqueous solution of K2CO3 (2×50 ml) and water (50 ml). The product was dried over Na2SO4 and evaporated. The residue was washed with ether and dried on the air to give ethyl 2-(4-chloro-3-fluorophenylamino)-2-oxoacetate (2′) (3.97 g, 78.6%) as a white powder; LC-MS (APCI+) m/z: calcd for C18H8CIFNO3: 245.03. found: 245 (M+H+).

1. customReaction mixture
2. customcontinued at room temperature
3. custom(RT)
4. customfor 6 h
5. washThe mixture was washed with 25% aqueous solution of K2CO3 (2×50 ml) and water (50 ml)
6. dry with materialThe product was dried over Na2SO4
7. customevaporated
8. washThe residue was washed with ether
9. customdried on the air