反应详情

温度

-78 °C

n-Butyllithium (1.6 M in hexane) (165 mL, 0.264 mmol) was added dropwise to a −78° C. solution of 1,4-dibromobenzene (60.1 g) in diethyl ether (500 mL). After stirring at −78° C. for 2 h, ethyl trifluoroacetate (40 g) was added dropwise and the mixture was allowed to warm to ambient temperature overnight. The reaction mixture was cooled to −20° C., quenched with saturated aqueous ammonium chloride and extracted with ether. The combined organic phases were washed with saturated aqueous sodium bicarbonate, dried (sodium sulfate) and concentrated in vacuo. Chromatography over silica eluting with petroleum ether/ethyl acetate (20:1) afforded the title compound.

1. temperatureto warm to ambient temperature overnight
2. temperatureThe reaction mixture was cooled to −20° C.
3. customquenched with saturated aqueous ammonium chloride
4. extractionextracted with ether
5. washThe combined organic phases were washed with saturated aqueous sodium bicarbonate
6. dry with materialdried (sodium sulfate)
7. concentrationconcentrated in vacuo