反应 #1103381
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07214475B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Freshly activated magnesium (8.5 g, 0.35 mol) was slowly added over a period of four hours to a solution of 1,4-dibromobenzene (80 g, 0.34 mol) in 200 mL of diethylether, keeping the temperature below 30° C. The reaction mixture was stirred for 8 hours and then slowly added to a mixture of tetrachlorosilane (100 mL, 0.87 mol) in diethylether (50 mL) within 12 hours. The mixture was stirred for 12 hours, and unreacted tetrachlorosilane and diethylether were removed in vacuum. The remaining liquid was fractionally distilled through a Vigreux column under reduced pressure to provide 4-bromophenyltrichlorosilane as an oil (350 μHg/85° C.-37 g/37%). 1HNMR(400 MHz, CDCl3): δ 7.69 (4H, dd). 13CNMR (100 MHz, CDCl3): δ 134.6, 131.9, 130.4, 128.2. GC-MS: 290 (M+). the temperature below 30° C The mixture was stirred for 12 hours unreacted tetrachlorosilane and diethylether were removed in vacuum The remaining liquid was fractionally distilled through a Vigreux column under reduced pressure
来源 ID: ord-d6650885382d4af098a51d0b1c5457b6