1,4-Dibromobenzene → HCID 131714345、化合物

HRID 463792

反応式

HRID 463792 の反応式
[CH3:1][Si:2]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([O:6][CH2:7][CH3:8])OCC.[Mg].Br[C:17]1[CH:22]=[CH:21][C:20](Br)=[CH:19][CH:18]=1>O1CCCC1>[CH3:1][SiH:2]([O:6][CH2:7][CH2:8][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:12]1[CH:11]=[CH:10][C:9]([SiH:2]([CH3:1])[O:6][CH2:7][CH2:8][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 78041,4-DibromobenzeneHCID 69891Benzene, (diethoxymethylsilyl)-HCID 5462224Magnesium

生成物 1

HCID 131714345HCID 131714345、化合物収率 147.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

21.0 g of methylphenyldiethoxysilane, 2.43 g of magnesium and 100 ml of tetrahydrofuran were charged into a 500-ml, three-necked flask provided with a stirrer, a cooler, and a dropping furnel and stirred in a nitrogen gas stream, while 100 ml of a tetrahydrofuran solution containing 11.8 g of p-dibromobenzene was dropwise added thereto from the dropping furnnal over about 3 hours. After the dropwise addition, the mixture was further stirred and refluxed for about 5 hours. After the refluxing, the resulting polymer was separated by filtration, and the solvent was removed therefrom by distillation. The residues were subjected to distillation under reduced pressure, whereby 15 g of p-bis(methylphenylethoxysilyl)benzene was obtained (yield: 78%, boiling point: 213°-215° C./3 mmHg).

後処理

  1. customprovided with a stirrer
  2. additionwas dropwise added
  3. additionAfter the dropwise addition
  4. temperaturerefluxed for about 5 hours
  5. customAfter the refluxing, the resulting polymer was separated by filtration
  6. customthe solvent was removed
  7. distillationby distillation
  8. distillationThe residues were subjected to distillation under reduced pressure

出典と根拠

ORDレコード
ord-c15d308d1cb54674a8ca0bbd3211a9d7
出典データセット
uspto-grants-1985_10
特許番号
US04544729

関連ノート

読み込み中…