反应详情

20.4 g of 6-hydroxy-2,5,7,8-tetramethyl-2-(4-nitrophenoxymethyl)chroman were dissolved in 60 ml of pyridine, and, while stirring, 30 ml of acetic anhydride were added dropwise at 10° C. The mixture was gradually restored to room temperature and then reacted for 1 hour at 30° C. The reaction mixture was cooled and then poured into ice-water and extracted with a 1:1 by volume mixture of benzene and cyclohexane. The extract was washed well with a 2% w/v aqueous solution of hydrochloric acid and then with water, after which it was dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure, giving the desired 6-acetoxy-2,5,7,8-tetramethyl-2-(4-nitrophenoxymethyl)chroman. Rf value on thin layer chromatography: 0.64 [silica gel; developing solvent; benzene and ethyl acetate=10:1 by volume]

1. customwas gradually restored to room temperature
2. customreacted for 1 hour at 30° C
3. temperatureThe reaction mixture was cooled
4. extractionextracted with a 1:1 by volume mixture of benzene and cyclohexane
5. washThe extract was washed well with a 2% w/v aqueous solution of hydrochloric acid
6. dry with materialwith water, after which it was dried over anhydrous sodium sulfate
7. customThe solvent was removed by evaporation under reduced pressure