反应详情

4.0 g of 1-(hydroxymethyl)-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ol prepared in Example 1-c was dissolved in 20 ml of tetrahydrofuran, and 1.2 ml of pyridine and 1.4 ml of acetic anhydride were added at room temperature, followed by stirring for 3 days. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate for two times. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:hexane=1:9), to give 3.5 g of the title compound as a colorless powder.

1. extractionthe mixture was extracted with ethyl acetate for two times
2. washThe organic layer was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was evaporated
5. customThe residue was purified
6. customseparated by silica gel column chromatography (ethyl acetate:hexane=1:9)