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

HRID 1349924ノート

反応式

HRID 1349924 の反応式
[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

参加物

5

反応物 3

HCID 78041,4-DibromobenzeneHCID 24816Silicon tetrachlorideHCID 5462224Magnesium

生成物 1

HCID 141374(4-Bromophenyl)trichlorosilane

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-d6650885382d4af098a51d0b1c5457b6
出典データセット
uspto-grants-2007_05
特許番号
US07214475B2

反応ノート

読み込み中…