反应详情

A mixture of 4-chloro-3-iodobenzotrifluoride (10.0 g), copper(I) iodide (124 mg), triphenylphosphine (428 mg), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (675 mg), propargyl alcohol (2.12 ml), diisopropylethylamine (22.6 ml) and tetrahydrofuran (180 ml) was stirred at room temperature for 15 hr. The reaction mixture was added to brine, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1-80:20) to give the object product (7.63 g) as a brown oil.

1. extractionthe mixture was extracted with ethyl acetate
2. washwashed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1-80:20)