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Volumn , Issue 5, 2004, Pages 978-983

Fast, high-yielding syntheses of silsesquioxanes using acetonitrile as a reactive solvent

Author keywords

Mass spectrometry; NMR spectroscopy; Silsesquioxanes; Solvent effects

Indexed keywords

ACETONITRILE; MASS SPECTROMETRY; ORGANIC SOLVENTS;

EID: 3843091660     PISSN: 14341948     EISSN: None     Source Type: Journal    
DOI: 10.1002/ejic.200300494     Document Type: Article
Times cited : (23)

References (25)
  • 15
    • 85153218165 scopus 로고    scopus 로고
    • note
    • Relative to silsesquioxane a7b3 (the yield is calculated by dividing the mass of product by the mass of silsesquioxane a7b3 that would be obtained if the reaction gave silsesquioxane a7b3 quantitatively).
  • 18
    • 85153276579 scopus 로고    scopus 로고
    • note
    • While the partial neutralisation of the HCl formed during the hydrolysis of trichlorosilanes might have a role in accelerating the formation of silsesquioxane precipitates, complete neutralisation is detrimental. A decrease of the yield (from 79 to 44%, as crude precipitate) was observed by performing the synthesis of cyclohexylsilsesquioxanes in the presence of triethylamine. This result indicates that the hydrolysis/condensation reactions in the absence of HCl are significantly slowed down from the beginning of the synthesis.
  • 21
    • 85153266990 scopus 로고    scopus 로고
    • note
    • 29Si NMR spectrum of the crude product.
  • 23
    • 85153262027 scopus 로고    scopus 로고
    • note
    • 1.5)] ppm]; the three less-intense peaks could not be assigned unambiguously among the remaining peaks of the silsesquioxane mixture.
  • 25
    • 85153202870 scopus 로고    scopus 로고
    • note
    • The synthesis conducted under reflux was performed on both 100- and 1000-mL scales, resulting in the formation of the same silsesquioxane mixture each time.


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.