(3-Bromophenyl)triphenylsilane synthesis

Yield:185626-73-7 95%

Reaction Conditions:

Stage #1:1,3-dibromobenzene with n-butyllithium in tetrahydrofuran at -78; for 1 h;
Stage #2:Triphenylsilyl chloride in tetrahydrofuran at 20; for 12 h;

Steps:

8
1,3-Dibromobenzene 20 g (84.77 mmol) was dissolved in THF 500 mL, and then cooled to a temperature of -78. n-BuLi 2.5M 33.9 mL(84.77 mmol) was slowly added thereinto, and then stirred at a temperature of -78 for 1 hour. Chlorotriphenylsilane ((C₆H₅)₃SiCl) 29.9 g was dissolved in THF 100 mL, and this solution was added into the above reaction mixture. The resultant mixture was slowly warmed to room temperature, and stirred for 12 hours. Then, extraction with EA, wash with distilled water and aqueous NaCl solution, drying over MgSO₄, distillation under reduced pressure, and recrystallization with MC-MeOH in the ratio of 1:10, were sequentially performed, thereby obtaining Compound 8-1 18 g(95 %).

References:

Rohm And Haas Electronic Materials Korea Ltd.;Kim, Chi Sik;Lee, Soo Yong;Kim, Young Gil;Lee, Hyo-Jung;Lee, Su Hyun;Kim, Hyun;Cho, Young Jun;Chang, Hoon;Lee, Kyung Joo;Kim, Bong-Ok;Kim, Sung-Min EP2857395, 2015, A1 Location in patent:Paragraph 0071

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