反应详情

温度

85 °C

To a mixture of 1-fluoro-2-nitrobenzene (485 μL, 4.6 mmol) and 2-amino-2-methyl-propionic acid tert-butyl ester hydrochloride (1.0 g, 5.1 mmol) in DMF (5 mL) was added Et3N (1.3 mL, 9.3 mmol). The mixture was heated at 85° 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 10% EtOAc in Hexane as the eluent to afford the desired 2-methyl-2-(2-nitro-phenylamino)-propionic acid tert-butyl ester (640 mg, 50%).

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 10% EtOAc in Hexane as the eluent