反应详情

温度

125 °C

Under nitrogen, 0.755 g (3.38 mmol) of palladium acetate, 2.05 g (6.75 mmol) of tri(ortho-tolyl)phosphine and 97.8 ml (0.708 mol) of triethylamine were added to a solution of 34.0 g (0.135 mol) of 5-bromo-2-(2-fluoro-phenyl) -pyridine in 2.2 l of acetonitrile. Then 23.38 ml (0.216 mol) of acrylic acid ethyl ester were added, and the mixture was shaken in an autoclave at 125° C. for 20 h. After cooling, the mixture was poured onto ice/water, the mixture stirred at 5 to 10° C. for 1 h, and the precipitated product was collected by filtration and purified by chromatography (silica gel, n-heptane/ethyl acetate 3:1). Yield: 24.3 g.

1. temperatureAfter cooling
2. additionthe mixture was poured onto ice/water
3. stirringthe mixture stirred at 5 to 10° C. for 1 h
4. filtrationthe precipitated product was collected by filtration
5. custompurified by chromatography (silica gel, n-heptane/ethyl acetate 3:1)