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双环笼状四配位硅的合成及其结构表征
Synthesis and Characterization of Caged Bicyclic Phosphorous Quadridentate Silicon Complex
【摘要】 研究了以SiO2为原料低温合成高反应活性的五配位硅酸酯,并与1-氧代-1-磷杂-2,6,7-三氧杂双环[2.2.2]-4-氯甲基辛烷反应合成出具有对称结构的双环笼状四配位硅,通过红外光谱、13C和29Si固体核磁共振、质谱等测试手段确定了其结构.热分析结果表明,双环笼状四配位硅在700℃的失重仅为19.98%,且炭层呈密实片层状,说明目标产物具有优异的热稳定性和成炭性质.
【Abstract】 A novel caged bicyclic phosphorous quadridentate silicon complex was synthesized by reaction of 1-oxo-1-phospha-4-chloromethyl-2,6,7-trioxabicyclo[2.2.2]octane with the pentacoordinate silicon com- plex, which was synthesized directly from SiO2 by non-carbothermal reduction. Structure of the synthesized substance was confirmed by FTIR, MS, 13C and 29Si MAS NMR spectra, while thermal analysis tests indi- cated that the target compound possessed exceptional thermal stability.
【关键词】 二氧化硅;
双环笼状四配位硅;
合成;
表征;
【Key words】 silica; caged bicyclic phosphorous quadridentate silicon complex; synthesis, charaterization;
【Key words】 silica; caged bicyclic phosphorous quadridentate silicon complex; synthesis, charaterization;
【基金】 国家自然科学基金(No.29974009)资助项目.
- 【文献出处】 有机化学 ,Chinese Journal of Organic Chemistry , 编辑部邮箱 ,2006年08期
- 【分类号】O627.41
- 【被引频次】10
- 【下载频次】303