反应详情

温度

80 °C

4-[1-Ethyl-1-(3-methyl-4-trifluoromethanesulfonyloxy-phenyl)-propyl]-2-methyl-benzoic acid methyl ester (11.20 g, 24.43 mmol) in DMF (100 ml) is added trimethylsilylacetylene (6.90 ml, 48.85 mmol), dichlorobis(triphenylphosphine) palladium (1.71 g, 2.44 mmol) and triethylamine (23.84 ml, 171 mmol) and heated to 80° C. overnight. The reaction mixture is concentrated and filtered through a pad of silica gel eluted with 10% EtOAc/Hexanes. The eluent is concentrated and chromatographed (330 g SiO2, 2% EtOAc/Hexanes) to yield the title compound (8.07 g, 81%) as an orange oil.

1. concentrationThe reaction mixture is concentrated
2. filtrationfiltered through a pad of silica gel
3. washeluted with 10% EtOAc/Hexanes
4. concentrationThe eluent is concentrated
5. customchromatographed (330 g SiO2, 2% EtOAc/Hexanes)