反应详情

Add bis(triphenylphosphine)palladium (II) dichloride (70 mg, 0.10 mmol), copper (I) iodide (38 mg, 0.20 mmol), and 3-ethynyl-5-methoxypyridine, (prepared as described in PREPARATION 10), (400 mg, 3.0 mmol) to a solution of 2-fluoro-5-iodobenzoic acid (0.53 g, 2.0 mmol) in triethylamine (4.2 mL, 30.0 mmol) and stir at room temperature for 1 h. Heat at 50° C. for 18 h. Cool to room temperature and concentrate. Purify by silica gel chromatography, eluting with 100:0 to 60:40 ethyl acetate:methanol. Triturate the resulting solid with 3:1 hexanes:methanol to give the title compound as an off-white solid (295 mg, 54%).

1. temperatureHeat at 50° C. for 18 h
2. temperatureCool to room temperature
3. concentrationconcentrate
4. customPurify by silica gel chromatography
5. washeluting with 100:0 to 60:40 ethyl acetate
6. customTriturate the resulting solid with 3:1 hexanes