1,4-Dibromobenzene → HCID 131714345, 화합물

HRID 463792

반응식

HRID 463792 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 131714345HCID 131714345, 화합물수율 147.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c15d308d1cb54674a8ca0bbd3211a9d7
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04544729

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