反应详情

温度

-78 °C

Into a solution of 1,3,5-tribromobenzene (9.0 g, 28.6 mmol) in diethyl ether (200 mL) was added n-butyllithium solution in hexane (2.5 M, 12 mL, 30.6 mmol) dropwise at −78° C. The reaction was stirred at this temperature for 30 minutes before a solution of chlorotriphenylsilane (9.27 g, 31.4 mmol) in diethyl ether (90 mL) was added dropwise. The reaction mixture was stirred at −78° C. for 1 hour, and then allowed to warm to room temperature and continue to stir overnight, and finally refluxed for 2 hours. After cooling to room temperature, the solid was filtered off. Upon evaporation of the solvent, the residue was purified by column chromatography on silica gel with hexane/DCM (9/1, v/v) as eluent to yield (3,5-dibromophenyl)triphenylsilane (4.0 g, 28%) as a white solid.

1. additionwas added dropwise
2. temperatureto warm to room temperature
3. stirringto stir overnight
4. temperaturefinally refluxed for 2 hours
5. temperatureAfter cooling to room temperature
6. filtrationthe solid was filtered off
7. customUpon evaporation of the solvent
8. customthe residue was purified by column chromatography on silica gel with hexane/DCM (9/1