反应详情

温度

45 °C

3,4,5-Trimethoxyphenylacetylene (1.80 g), ethyl 2-chloroisonicotinate (2.08 g) and copper iodide (71 mg) were dissolved in a mixed solvent of DMF (4 mL) and triethylamine (8 mL), and to the solution bis-(triphenylphosphine)palladium dichloride (0) (131 mg) was added, and the mixture was stirred at 45° C. for 4 hours under an argon atmosphere. The reaction mixture was diluted with ethyl acetate, washed with 2 M hydrochloric acid, water and saturated brine, dried over anhydrous sodium sulfate. After concentrating the reaction mixture under reduced pressure, the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1 to 3:1) to obtain the title compound.

1. washwashed with 2 M hydrochloric acid, water and saturated brine
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationAfter concentrating the reaction mixture under reduced pressure
4. customthe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1 to 3:1)