反应详情

温度

70 °C

Add 1-ethynyl-3-methoxybenzene (0.56 g, 4.22 mmol) to a mixture of 3,5-dibromopyridine (1.00 g, 4.22 mmol), bis(triphenylphosphine)palladium (II) dichloride (0.06 g, 0.08 mmol) and copper (I) iodide (0.03 g, 0.17 mmol) in triethylamine (8 mL) and heat at 70° C. for 2 h. Cool to room temperature, dilute with ethyl acetate and an aqueous saturated solution of ammonium chloride, and separate the layers. Wash the organic layer with an aqueous saturated solution of sodium chloride, dry (magnesium sulfate), filter and concentrate. Purify the resulting residue by silica gel chromatography, eluting with 2.5% ethanol in 50:50 chloroform/hexanes, to give the title compound (0.86 g, 71%).

1. temperatureCool to room temperature
2. customan aqueous saturated solution of ammonium chloride, and separate the 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 the resulting residue by silica gel chromatography
8. washeluting with 2.5% ethanol in 50:50 chloroform/hexanes