1,4-Dibromobenzene → (4-Bromophenyl)trichlorosilane

HRID 1349924노트

반응식

HRID 1349924 반응식
[Mg].[Br:2][C:3]1[CH:8]=[CH:7][C:6](Br)=[CH:5][CH:4]=1.[Cl:10][Si:11](Cl)([Cl:13])[Cl:12]>C(OCC)C>[Br:2][C:3]1[CH:8]=[CH:7][C:6]([Si:11]([Cl:13])([Cl:12])[Cl:10])=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 78041,4-DibromobenzeneHCID 24816Silicon tetrachlorideHCID 5462224Magnesium

생성물 1

HCID 141374(4-Bromophenyl)trichlorosilane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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+).

후처리

  1. customthe temperature below 30° C
  2. stirringThe mixture was stirred for 12 hours
  3. customunreacted tetrachlorosilane and diethylether were removed in vacuum
  4. distillationThe remaining liquid was fractionally distilled through a Vigreux column under reduced pressure

출처 및 근거

ORD 기록
ord-d6650885382d4af098a51d0b1c5457b6
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214475B2

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