反应详情

To a stirred solution of 2-chloro-4-(3-chloro-4-methyl-phenoxy)-benzonitrile (14.41 g) in CCl4 (100 ml) under argon were added N-bromosuccinimide (9.5 g) and dibenzoylperoxide (1.38 g). The mixture was heated to reflux for 2.5 h. After cooling to room temperature, the mixture was filtered. The filter cake was washed with cyclohexane. The combined filtrate was concentrated to dryness to give the crude product (19.75 g) as a light orange solid. Part of the product was purified by repeated chromatography (SiO2, cyclohexane/ethyl acetate 1:0=>4:1) to give the title compound as an off-white solid (3.27 g).

1. temperatureThe mixture was heated
2. temperatureto reflux for 2.5 h
3. filtrationthe mixture was filtered
4. washThe filter cake was washed with cyclohexane
5. concentrationThe combined filtrate was concentrated to dryness
6. customto give the crude product (19.75 g) as a light orange solid
7. customPart of the product was purified by repeated chromatography (SiO2, cyclohexane/ethyl acetate 1:0=>4:1)