反应详情

To 1,3-benzenedimethanol (5.10 g, 36.91 mmol) in dichloromethane (70 ml) was added at 0° C. triethylamine (7.47 g, 73.82 mmol), 4-dimethyl-aminopyridine (451 mg, 3.61 mmol) and t-butyldimethylchlorosilane (5.56 g, 36.91 mmol) successively, and the mixture was stirred for 20 hours at room temperature. Thereto was added a saturated ammonia solution and the mixture was extracted with ethyl acetate and separated by a separating funnel. The organic layer was washed with water and saturated brine, dried over magnesium sulfate and filtered. The solvent was removed in vacuo and the residue was purified by silica gel column chromatography to give the subject compound (4.23 g, 45%).

1. extractionthe mixture was extracted with ethyl acetate
2. customseparated by a separating funnel
3. washThe organic layer was washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customThe solvent was removed in vacuo
7. customthe residue was purified by silica gel column chromatography