反应详情

温度

60 °C

Add bis(triphenylphosphine)palladium (II) dichloride (77 mg, 0.1 mmol), copper (I) iodide (44 mg, 0.23 mmol), and 3-ethynyl-5-methoxypyridine (300 mg, 2.3 mmol), (prepared as described in PREPARATION 10), to a solution of 2-fluoro-5-iodobenzonitrile (670 mg, 2.7 mmol) in triethylamine (3.4 mL, 34 mmol) and heat at 60° C. for 2.75 h. Cool to room temperature and concentrate. Purify the residue by silica gel chromatography, eluting with 100:0 to 80:20 dichloromethane/ethyl acetate followed by a second silica gel chromatography, eluting with 75:25 to 60:40 hexanes:ethyl acetate to give the title compound as a white solid (510 mg, 90%).

1. temperatureCool to room temperature
2. concentrationconcentrate
3. customPurify the residue by silica gel chromatography
4. washeluting with 100:0 to 80:20 dichloromethane/ethyl acetate
5. washeluting with 75:25 to 60:40 hexanes