反应详情

Under an argon atmosphere, ethyldiisopropylamine (7.0 mL), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (518 mg), xantphos (578 mg), and 3-trifluoromethylthiophenol (3.56 g) were added at room temperature into a solution of 4-bromo-2-fluorobenzaldehyde (4.06 g) in 1,4-dioxane (42 mL), and the resultant solution was heated to reflux for 5 hours. To the reaction solution added water, extracted with ethyl acetate, washed with water and saturated brine in that order, and then dried over anhydrous sodium sulfate. The solvent was evaporated, and the resultant residue was purified by silica gel column chromatography (hexane:ethyl acetate=30:1) to obtain the target product (4.08 g) as a colorless oil.

1. temperatureto reflux for 5 hours
2. extractionextracted with ethyl acetate
3. washwashed with water and saturated brine in that order
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated
6. customthe resultant residue was purified by silica gel column chromatography (hexane:ethyl acetate=30:1)