反应详情

温度

150 °C

A mixture of {3-[(4-{[(1,1-dimethylethyl)oxy]carbonyl}-1-piperazinyl)methyl]phenyl}boronic acid (1 g), 3-bromobenzonitrile (0.56 g), potassium carbonate (1.725 g) and tetrakis triphenylphosphine palladium (180 mg) in dioxan/water (3:1, 4 mL) was sealed in a tube and heated at 150° C. for 15 minutes in a microwave vessel. After cooling to room temperature, the reaction mixture was then diluted with water (25 mL) and extracted with ethyl acetate (2×25 mL). The combined organic phases were dried (MgSO4) and concentrated under vacuum. The resulting crude residue was further purified by flash column chromatography on silica (100 g) to give the title compound (0.9 g) (purity ca 75%). LC/MS: m/z, 378 (M+H), 2.57 min.

1. customwas sealed in a tube
2. temperatureAfter cooling to room temperature
3. extractionextracted with ethyl acetate (2×25 mL)
4. dry with materialThe combined organic phases were dried (MgSO4)
5. concentrationconcentrated under vacuum
6. customThe resulting crude residue was further purified by flash column chromatography on silica (100 g)