反应详情

温度

70 °C

Add 1-ethynyl-3-fluorobenzene (250 mg, 2.11 mmol) to a mixture of 3,5-dibromopyridine (500 mg, 2.11 mmol) in triethylamine (4 mL) containing bis(triphenylphosphine)palladium (II) dichloride (28 mg, 0.04 mmol) and copper (I) iodide (15 mg, 0.08 mmol) and heat at 70° C. for 2 h. Cool to room temperature, dilute with ethyl acetate and an aqueous solution of ammonium chloride and separate the resulting layers. Wash the organic layer with an aqueous saturated solution of sodium chloride, dry (magnesium sulfate), filter and concentrate. Purify by silica gel chromatography, eluting with 0.5% ethanol in 50:50 dichloromethane:hexanes to give the title compound (160 mg, 28%).

1. temperatureCool to room temperature
2. customan aqueous solution of ammonium chloride and separate the resulting layers
3. washWash the organic layer with an aqueous saturated solution of sodium chloride
4. dry with materialdry (magnesium sulfate)
5. filtrationfilter
6. concentrationconcentrate
7. customPurify by silica gel chromatography
8. washeluting with 0.5% ethanol in 50:50 dichloromethane