Synthesis
a) Under a dry nitrogen atmosphere, 10.81 g (50 mmol) of 1,4-dibromobenzene was dissolved in 400 mL of anhydrous tetrahydrofuran (THF) and the solution was cooled to -78 °C. Subsequently, 20 mL (50 mmol) of hexane solution of n-butyllithium (n-BuLi) was slowly added dropwise, keeping the reaction temperature at -78 °C. After the dropwise addition, the reaction mixture was continued to be stirred at -78 °C for 1 hour. Then, 6.3 g (25 mmol) of diphenyl dichlorosilane dissolved in 80 mL of anhydrous THF was slowly added dropwise, and upon completion of the dropwise addition, the reaction mixture was allowed to slowly warm to room temperature and stirred overnight. After completion of the reaction, the solvent was evaporated to dryness using a rotary evaporator and the crude product obtained was purified by recrystallization from toluene. Ultimately, 10 g (0.021 mol) of bis(4-bromophenyl)diphenylsilane was obtained from recrystallization from n-butanol in 81% yield.
References
[1] Patent: KR2016/69021, 2016, A. Location in patent: Paragraph 0191-0193
[2] Patent: CN108129386, 2018, A. Location in patent: Paragraph 0155; 0157; 0158
[3] Patent: CN103804409, 2016, B. Location in patent: Paragraph 0026; 0056-0057
[4] Patent: US2012/305851, 2012, A1. Location in patent: Page/Page column 66-67
[5] Journal of Materials Chemistry C, 2014, vol. 2, # 25, p. 5019 - 5027
