反应详情

A mixture of N-[3,5-bis(trifluoromethyl)phenyl]-2-hydroxy-5-iodo-benzamide (475 mg, 1 mmol), styrene (130 mg, 1.25 mmol), palladium acetate (4.5 mg, 0.02 mmol), tris(ortho-tolyl)phosphine (12.2 mg, 0.04 mmol), diisopropylamine (388 mg, 3 mmol) and N,N-dimethylformamide (2 mL) was refluxed for 8 hours. After cooling, water was added to the reaction mixture, and it was extracted with ethyl acetate. After the ethyl acetate layer was washed with water and brine, dried over anhydrous magnesium sulfate and concentrated, the residue was purified by column chromatography on silica gel (hexane-isopropyl ether: 2/1→1/1) to give the title compound (173 mg, 38.3%) as a pale yellow solid.

1. temperaturewas refluxed for 8 hours
2. temperatureAfter cooling
3. extractionwas extracted with ethyl acetate
4. washAfter the ethyl acetate layer was washed with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customthe residue was purified by column chromatography on silica gel (hexane-isopropyl ether: 2/1→1/1)