反应详情

温度

150 °C

To a mixture of tert-butyl (2-fluoro-5-aminophenyl)carbamate (2.02 g, 8.93 mmol), K2CO3 (2.47 g, 17.86 mmoll) and NaI (4.02 g, 26.79 mmol) in DMF (60 mL) was added 2,2′-dichlorodiethyl ether (1.28 g, 8.93 mmol) slowly at 150° C. under N2. The reaction was heated at 150° C. overnight, then cooled to rt, poured into water (200 mL) and extracted with CH2Cl2 (200 mL×2). The combined organic phases were washed with water (200 mL×2) and brine (200 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=4:1) to give the title compound as a yellow solid (0.93 g, 35%).

1. temperaturecooled to rt
2. extractionextracted with CH2Cl2 (200 mL×2)
3. washThe combined organic phases were washed with water (200 mL×2) and brine (200 mL)
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=4:1)