反应详情

温度

140 °C

To a solution of 2-fluoro-4-nitroaniline (2.34 g, 15.0 mmol) in DMF (30 mL) were added K2CO3 (4.2 g, 30.4 mmol), KI (0.5 g, 3.01 mmol) and 1-(2-bromoethyl)adamantane (3.65 g, 15.0 mmol) and the mixture was stirred at 140° C. for 12 h. The mixture was then cooled to rt and filtered. The filtrate was diluted with 150 mL of DCM and washed with water (50 mL×3), brine (150 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=8:1) to give the title compound as a yellow solid (477 mg, 10%).

1. temperatureThe mixture was then cooled to rt
2. filtrationfiltered
3. additionThe filtrate was diluted with 150 mL of DCM
4. washwashed with water (50 mL×3), brine (150 mL)
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=8:1)