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Dichlorodiphenylsilane → Trimethylsiloxydiphenylchlorosilane

HRID 2379903
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HRID 2379903 반응식
[C:1]1([Si:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)(Cl)[Cl:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:16][Si:17]([CH3:20])([CH3:19])[OH:18].C(N(CC)CC)C>O1CCCC1>[CH3:16][Si:17]([CH3:20])([CH3:19])[O:18][Si:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6627DichlorodiphenylsilaneHCID 8471TriethylamineHCID 66110Trimethylsilanol

생성물 1

HCID 19417892Trimethylsiloxydiphenylchlorosilane수율 71.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The following were ingredients were introduced into a stirrer-equipped four-neck flask: 164.8 g (651.2 mmol) diphenyldichlorosilane and 300 mL tetrahydrofuran. The resultant mixture was stirred at room temperature while a mixture of 60 g (542.7 mmol) of 81.4% pure trimethylsilanol and 65.9 g (651.2 mmol) of triethylamine was added dropwise. Stirring at room temperature was continued for an additional hour following completion of the addition, at which time the salt formed as a by-product of the reaction was removed by filtration. The filtrate was then distilled under reduced pressure to yield 118.7 g of a fraction boiling at 136.5° C.-142° C. under of 2 mm Hg, equivalent to a 71.4% yield of trimethylsiloxydiphenylchlorosilane. Analysis of this product by gas chromatography (GLC), nuclear magnetic resonance (NMR), and infrared spectrochemical analysis (IR) confirmed it to be trimethylsiloxydiphenylchlorosilane with the following structural formula. ##STR6##

후처리

  1. additionwere introduced into a stirrer-equipped four-neck flask
  2. additionwas added dropwise
  3. waitwas continued for an additional hour
  4. additioncompletion of the addition
  5. customat which time the salt formed as a by-product of the reaction
  6. customwas removed by filtration
  7. distillationThe filtrate was then distilled under reduced pressure

출처 및 근거

ORD 기록
ord-d4d30c271a5a413ab29ed7fb832db57c
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05364896

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