反应详情

温度

90 °C

To a mixture of 1-fluoro-2-nitrobenzene (450 □L, 4.3 mmol) and (1-amino-cyclohexyl)-acetic acid methyl ester (880 mg, 5.2 mmol) in DMF (5 mL) was added DIPEA (1.0 mL, 5.7 mmol). The mixture was heated at 90° C. for 16 hours. The reaction mixture was allowed to cool to room temperature, diluted with EtOAc (50 mL) and washed with H2O (50 mL×3). The organic layer was dried over sodium sulfate and concentrated. The resulting residue was purified by CombiFlash with 20% EtOAc in Hexane as the eluent to afford the desired [1-(2-nitro-phenylamino)-cyclohexyl]-acetic acid methyl ester (230 mg, 19%).

1. temperatureto cool to room temperature
2. washwashed with H2O (50 mL×3)
3. dry with materialThe organic layer was dried over sodium sulfate
4. concentrationconcentrated
5. customThe resulting residue was purified by CombiFlash with 20% EtOAc in Hexane as the eluent