反应详情

温度

100 °C

To a solution of ethyl 3-methoxy-4-trifluoromethane-sulfonyloxybenzoate (3.95 g), 4-methylphenylacetylene (1.54 g) and triethylamine (5.0 ml) in DMF (40 ml) was added bistriphenylphosphine palladium dichloride (0.25 g), and the mixture was stirred at 100° C. for 3 hours and then cooled to room temperature. To the mixture was added water, and the mixture was extracted with diethylether. The organic layer was washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the mixture was concentrated, and the residue was purified with column chromatography (ethyl acetate/hexane=1:9) and recrystallized from ethyl acetateihexane to give pale yellow crystals of ethyl 3-methoxy-4-[2-(4-methylphenyl)ethynyl]-benzoate (2.02 g).

1. temperaturecooled to room temperature
2. extractionthe mixture was extracted with diethylether
3. washThe organic layer was washed with saturated brine
4. dry with materialdried with magnesium sulfate
5. concentrationUnder reduced pressure, the mixture was concentrated
6. customthe residue was purified with column chromatography (ethyl acetate/hexane=1:9)
7. customrecrystallized from ethyl acetateihexane