反应详情

温度

80 °C

Add phenylacetylene (0.460 mL, 4.2 mmol), copper (I) iodide (0.072 g, 0.38 mmol) and bis(triphenylphosphine)palladium (II) dichloride (0.133 g, 0.19 mmol) to a solution of 3-bromo-5-methylpyridine, (prepared essentially as described in PREPARATION 1), (0.654 g, 3.8 mmol) in degassed triethylamine (20 mL) and stir under nitrogen at 80° C. for 16 h. Cool the reaction mixture to room temperature, filter through diatomaceous earth, wash with ethyl acetate, and concentrate. Purify the residue by silica gel chromatography, eluting with 80:20 hexanes:ethyl acetate, to give the title compound as a brown oil (0.398 g, 54%).

1. custom(prepared essentially
2. temperatureCool the reaction mixture to room temperature
3. filtrationfilter through diatomaceous earth
4. washwash with ethyl acetate
5. concentrationconcentrate
6. customPurify the residue by silica gel chromatography
7. washeluting with 80:20 hexanes