反应详情

4-Methoxyphenylboronic acid (10.15 g, 66.8 mmol), tripotassium phosphate hydrate (77.6 g, 278.3 mmol) and tetrakis(triphenylphosphine)palladium(0) (1.93 g, 1.67 mmol, 3 mol %) were added to a solution of 6-methoxy-1-(2-propenyl)-2-naphthyl trifluoromethanesulfonate (19.3 g, 55.66 mmol) in dioxane (300 ml), followed by heating under reflux for 8 hours under argon atmosphere. Water was added to the reaction mixture, which was then extracted with ethyl acetate, washed with saturated aqueous sodium chloride, and dried over anhydrous sodium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/9), followed by recrystallization from hexane, to give 6-methoxy-2-(4-methoxyphenyl)-1-(2-propenyl)naphthalene (12.65 g, Yield 75%).

1. temperatureby heating
2. temperatureunder reflux for 8 hours under argon atmosphere
3. extractionwas then extracted with ethyl acetate
4. washwashed with saturated aqueous sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. distillationAfter distilling off the solvent
7. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/9)
8. customfollowed by recrystallization from hexane