反应详情

温度

80 °C

To 28 ml of a 1M solution of trichloroborane at −5° C. are added 5.6 g of 4-chloroaniline dissolved in 30 ml of 1,2-dichloroethane. After 45 minutes at +15° C., 3.8 g of 2,5-dichlorobenzonitrile and 5 g of gallium trichloride are introduced and the mixture is refluxed for 3 hours. At room temperature, the resulting mixture is hydrolysed with 2M hydrochloric acid solution and maintained at 80° C. for 2 hours. The reaction medium is taken up in ethyl acetate and washed with water. The organic phase is dried over anhydrous sodium sulfate and concentrated. The residue is chromatographed on a column of silica gel, eluting with a cyclohexane/dichloromethane gradient to give 6.38 g of the expected product.

1. temperaturethe mixture is refluxed for 3 hours
2. customAt room temperature
3. washwashed with water
4. dry with materialThe organic phase is dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe residue is chromatographed on a column of silica gel
7. washeluting with a cyclohexane/dichloromethane gradient