1,4-Dibromobenzene → HCID 131714345, Verbindung

HRID 463792

Reaktionsgleichung

Reaktionsgleichung von HRID 463792
[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

Komponenten

5

Edukt 3

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

Produkt 1

HCID 131714345HCID 131714345, VerbindungAusbeute 147,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-c15d308d1cb54674a8ca0bbd3211a9d7
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04544729

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