反应详情

In a nitrogen atmosphere, 12 g (35.7 mmol) of 9,10-dibromoanthracene, and 300 ml of tetrahydrofuran (THF) were added to a round-bottom flask. Next, 14.4 ml (35.7 mmol, 2.5M) of n-butyl lithium was added dropwise slowly into the round-bottom flask at −78° C. After mixing and reacting for 30 min, 12 g (40.7 mmol) triphenylsilyl chloride with 50 ml THF were added dropwise slowly into the round-bottom flask at −78° C. After reacting at room temperature for 24 hours, the resulting mixture was subjected to extraction with a mixed solvent (ethyl acetate:H2O), dried over anhydrous MgSO4, filtered, and condensed, then the crude product was purified by column chromatography (n-hexane/acetyl acetate=15/1), A 9.0 g of pure 9-bromo-10-triphenysilyl anthracene was collected.

1. additionAfter mixing
2. waitAfter reacting at room temperature for 24 hours
3. extractionthe resulting mixture was subjected to extraction with a mixed solvent (ethyl acetate:H2O)
4. dry with materialdried over anhydrous MgSO4
5. filtrationfiltered
6. customcondensed
7. customthe crude product was purified by column chromatography (n-hexane/acetyl acetate=15/1)
8. customA 9.0 g of pure 9-bromo-10-triphenysilyl anthracene was collected