反应详情

A mixture of 2-chloro-5-iodo-benzoic acid methyl ester (3.5 g, 12 mmol), dichlorobis(triphenylphosphino)palladium (II) (0.04 g, 0.06 mmol), triphenylphosphine (0.06 g, 0.24 mmol), copper iodide (0.05 g, 0.24 mmol), (trimethylsilyl)acetylene (1.9 g, 19.2 mmol) in triethylamine (40 mL) was heated at reflux for 12 h. The mixture was concentrated in vacuo, diluted with ethyl acetate (150 mL) and washed sequentially with 10% aqueous citric acid, water, and brine. The organic solution was dried, filtered and concentrated in vacuo to afford the title compound (3.14 g).

1. temperaturewas heated
2. temperatureat reflux for 12 h
3. concentrationThe mixture was concentrated in vacuo
4. additiondiluted with ethyl acetate (150 mL)
5. washwashed sequentially with 10% aqueous citric acid, water, and brine
6. customThe organic solution was dried
7. filtrationfiltered
8. concentrationconcentrated in vacuo