反应详情

To a mixture of 2-fluoro-4-iodotoluene (0.94 g, 4.0 mmol) in CCl4 (40 mL) were added BPO (0.02 g, 0.08 mmol) and NBS (0.78 g, 4.4 mmol) under N2. The reaction mixture was refluxed for 5 h, then cooled and concentrated in vacuo. To the residue was added a solution of methylpiperazine (2.00 g, 20 mmol) in EtOH (40 mL) under N2. The mixture was stirred at rt overnight and concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=10:1) to give the title compound as a white solid (0.69 g, 52%).

1. temperatureThe reaction mixture was refluxed for 5 h
2. temperaturecooled
3. concentrationconcentrated in vacuo
4. concentrationconcentrated in vacuo
5. customThe resulting residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=10:1)