反应详情

温度

80 °C

To a suspension of 4-(4-n-octylphenyl)phenol (2.82 g) in 1,2-dichloroethane (40 ml) is added a 2M borone trichloride - 1,2-dichloroethane solution (6 ml) under ice cooling, and thereto are further added methyl thiocyanate (0.82 ml) and aluminum chloride (1.33 g). The mixture is stirred at room temperature until aluminum chloride is dissolved, and is further stirred at 80° C. for 3 hours. After cooling, 4N aqueous sodium hydroxide solution (33 ml) is added to the reaction mixture, and the mixture is stirred at 75°-80° C. for 30 minutes. After cooling, the reaction mixture is washed with methylene chloride, and the aqueous layer is adjusted to pH 2 with 6N hydrochloric acid and then extracted with ether. The extract is dried and then ether is distilled off under reduced pressure. The crude crystal thus obtained is purified by silica gel column chromatography to give 4-(4-n-octylphenyl)-2-cyanophenol (2.03 g) of the following formula: ##STR32##

1. additionis added a 2M
2. dissolutionis dissolved
3. temperatureAfter cooling
4. stirringthe mixture is stirred at 75°-80° C. for 30 minutes
5. temperatureAfter cooling
6. washthe reaction mixture is washed with methylene chloride
7. extractionextracted with ether
8. customThe extract is dried
9. distillationether is distilled off under reduced pressure
10. customThe crude crystal thus obtained
11. customis purified by silica gel column chromatography