反应详情

温度

80 °C

2,7-di bromo fluorene (25 g, 77 mmol), octylbromide (44.7 g, 0.596 mols), sodium hydroxide (37.5 g, 0.937 mols), and tetrabutyl ammonium bromide (0.5 g, 1.55 mmol) were dissolved in dimethyl sulfoxide (75 ml)-water (37.5 ml) mixed solvent. It was kept warm at 80° C. for 6 hours. After cooling, toluene (100 ml) and water (100 ml) were added, and the organic layer was partitioned. The organic layer is washed with water, 3% hydrochloric acid, and water, and then dehydrated with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the crude product was purified by silica-gel chromatography, and 2,7-dibromo-9,9-dioctylfluorene was obtained. (Amount: 26.85 g, yield: 79%)

1. additionmixed solvent
2. temperatureAfter cooling
3. customthe organic layer was partitioned
4. washThe organic layer is washed with water, 3% hydrochloric acid, and water
5. distillationThe solvent was distilled off under reduced pressure
6. customthe crude product was purified by silica-gel chromatography