反应详情

4-t-Butyldimethylsilyloxymethyl-2,3'-dimethylbenzhydrol (6 g, 16.8 millimol) was dissolved in pyridine (10 ml), and thereto was added dimethylaminopyridine (200 mg, 1,6 millimol), and the mixture was cooled with ice. To the mixture were added acetylchloride (1.54 g, 19.6 millimol) and methylene chloride (10 ml). The mixture was returned to room temperature, and stirred for 2 hours. After adding water, the mixture was extracted with ethyl acetate, the organic layer was washed with in turn dil. hydrochloric acid, water and saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate. The solvent was distilled away to give the title compound (6.9 g, 16.6 millimol, 99%).

1. temperaturethe mixture was cooled with ice
2. customwas returned to room temperature
3. extractionthe mixture was extracted with ethyl acetate
4. washthe organic layer was washed with in turn dil. hydrochloric acid, water and saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled away