反应详情

9-bromo-10-triphenysilyl anthracene (4 g, 7.8 mmol), 2-naphthylboronic acid (1.6 g, 9.4 mmol) and K2CO3 (1.5 g,15.6 mmol) were dissolved in the solvent mixture of 50 mL ethylene glycol dimethyl ether and 75 mL water. The stirred solution was added tetrakis (triphenylphosphine) palladium (0) and the mixture refluxed under N2 for 16 hours. The reaction mixture was cooled and the water extracted with acetyl acetate three times. The combined organic phase was washed with portions of brine. The organic layer was then dried with MgSO4, filtered, and evaporated of solvent. The crude material was purified by column chromatography (n-hexane/acetyl acetate=10/1) to give 9-(2-naphthyl)-10-triphenysilyl anthracene (Compound 2), the reaction was following:

1. temperaturethe mixture refluxed under N2 for 16 hours
2. temperatureThe reaction mixture was cooled
3. extractionthe water extracted with acetyl acetate three times
4. washThe combined organic phase was washed with portions of brine
5. dry with materialThe organic layer was then dried with MgSO4
6. filtrationfiltered
7. customevaporated of solvent
8. customThe crude material was purified by column chromatography (n-hexane/acetyl acetate=10/1)