反应详情

温度

60 °C

Add bis(triphenylphosphine)palladium (II) dichloride (110 mg, 0.15 mmol), copper (I) iodide (57 mg, 0.30 mmol), and 3-ethynyl-5-methoxypyridine, (prepared as described in PREPARATION 10), (400 mg, 3.0 mmol) to a solution of 2-chloro-1-fluoro-4-iodobenzene (0.46 mL, 3.6 mmol) in triethylamine (6.3 mL, 45.0 mmol) and heat at 60° C. for 5 h. Cool to room temperature and concentrate. Purify the residue by silica gel chromatography, eluting with a gradient of 100:0 to 80:20 dichloromethane:ethyl acetate, followed by a second silica gel chromatography, eluting with 67:33 to 60:40 hexanes:ethyl acetate, to give the title compound as a white solid (730 mg, 93%).

1. temperatureCool to room temperature
2. concentrationconcentrate
3. customPurify the residue by silica gel chromatography
4. washeluting with a gradient of 100:0 to 80:20 dichloromethane
5. washeluting with 67:33 to 60:40 hexanes