反应详情

温度

30 °C

450 ml of 2N sodium hydroxide were added to the toluene filtrate at room temperature and gradually heated to reflux. The reaction was heated at reflux for 41/2 hours. The reaction mixture was cooled to 0° to 5° C. by an ice-water bath whereupon a thick precipitate formed consisting of the intermediate sodium 4-(3,5-di-tert-butyl-4-hydroxybenzoyloxy)-3,5-di-tert-butylbenzoate. 70 ml of concentrated aqueous hydrochloric acid was gradually added dropwise with cooling at 30° C. 150 ml of ether was added with stirring to the reaction mixture at 20° to 25° C. The aqueous phase was separated and the organic phase washed with two 100 ml portions of water. The separated organic phase was then dried over anhydrous sodium sulfate. The residue was isolated from the organic phase by evaporation of the solvent initially at about 20 mm Hg. pressure and finally at 0.5 mm Hg.

1. temperaturegradually heated to reflux
2. temperatureThe reaction was heated
3. temperatureat reflux for 41/2 hours
4. temperatureThe reaction mixture was cooled to 0° to 5° C. by an ice-water bath whereupon a thick precipitate
5. customformed
6. customThe aqueous phase was separated
7. washthe organic phase washed with two 100 ml portions of water
8. dry with materialThe separated organic phase was then dried over anhydrous sodium sulfate
9. customThe residue was isolated from the organic phase by evaporation of the solvent initially at about 20 mm Hg