反应详情

4-methyl-3-(trifluoromethyl)benzonitrile (10 g, 54 mmol) was dissolved in 200 mL of carbon tetrachloride and treated with N-bromosuccinimide (10.5 g, 59 mmol) and benzoyl peroxide (1.3 g, 0.54 mmol). The reaction mixture was heated to reflux temperature and stirred for one week. Then, 80 mL of water was added and the layers were separated. The aqueous layer was extracted with methylene chloride (2×50 mL). The combined organic layers were washed with water (2×50 mL), dried over magnesium sulfate, and concentrated to provide 4-(bromomethyl)-3-(trifluoromethyl)benzonitrile (14 g, 53 mmol) as a yellow oil which was used in the next step without further purification.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux temperature
3. customthe layers were separated
4. extractionThe aqueous layer was extracted with methylene chloride (2×50 mL)
5. washThe combined organic layers were washed with water (2×50 mL)
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated