反应详情

温度

80 °C

1.0 ml (15.0 mmol) of 2-chloroethanol is added to a solution of 3.38 g (10.0 mmol) of 5,7-di-tert-butyl-3-(4-hydroxyphenyl)benzofuran-2-one in 30 ml of 1N sodium hydroxide solution heated to 80° C. The reaction mixture is then maintained at 80° C. for 2 hours, 50 ml of 1N hydrochloric acid are added, stirring is continued for 1 hour, the mixture is cooled, and the product is extracted with dichloromethane. The organic phases are washed with water, combined, dried over sodium sulfate and concentrated on a vacuum rotary evaporator. Crystallization of the residue from 8 ml of ethanol and 2 ml of water gives 2.34 g (61%) of 5,7-di-tert-butyl-3-[4-(2-hydroxyethoxy)phenyl]-benzofuran-2-one m.p. 132°-135° C. (compound (105), Table 1).

1. temperatureThe reaction mixture is then maintained at 80° C. for 2 hours
2. temperaturethe mixture is cooled
3. extractionthe product is extracted with dichloromethane
4. washThe organic phases are washed with water
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated on a vacuum rotary evaporator
7. customCrystallization of the residue from 8 ml of ethanol and 2 ml of water