反应详情

(4′-Bromobiphenyl-4-yl)methanol (1.2 g, 4.6 mmol) was dissolved in tetrahydrofuran (20 mL), and methyl iodide (0.97 g, 6.8 mmol), and then sodium hydride (63%, 0.26 g, 6.8 mmol) were added under a nitrogen atmosphere at 4° C., followed by stirring at room temperature for 30 minutes. A saturated aqueous ammonium chloride solution was added to the reaction solution, followed by extraction with ethyl acetate. After the solvent was distilled off under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/dichloromethane), and a fraction corresponding to the Rf value=0.50 (hexane/dichloromethane=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (1.2 g, 4.3 mmol) as a white solid (yield 95%).

1. extractionfollowed by extraction with ethyl acetate
2. distillationAfter the solvent was distilled off under reduced pressure
3. customthe resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/dichloromethane)
4. concentrationa fraction corresponding to the Rf value=0.50 (hexane/dichloromethane=1/1) by thin layer chromatography was concentrated under reduced pressure