Synthesis and reactivity of bis(triethoxysilyl)methane, tris(triethoxysilyl)methane and some derivatives
作者:Robert J.P. Corriu、Michel Granier、Gérard F. Lanneau
DOI:10.1016/s0022-328x(98)00365-9
日期:1998.7
Syntheses of new poly(trifunctional-silyl)alkanes, which are potent coupling agents of hybrid organic–inorganic materials have been thoroughly examined. Optimization of the Benkeser reaction using chloroform, trichlorosilane and tri-n-butylamine (respective ratios 1:4.5:3) afforded bis(trichlorosilyl)methane isolated as bis(triethoxysilyl)methane after ethanolysis (overall yield 60%). With nine equivalents
新的聚(三官能甲硅烷基)烷烃是有机-无机杂化材料的有效偶联剂,其合成已得到全面研究。在使用benkeser反应氯仿,三氯硅烷的优化和三- Ñ丁胺(各自的比例1:4.5:3)纯化,得到双(三氯甲硅烷基)甲烷分离为双(三乙氧基)乙醇解后(总产率60%)的甲烷。用九当量的三氯硅烷,优先形成三(三氯甲硅烷基)甲烷,将其分离为三(三乙氧基甲硅烷基)甲烷(收率30%)。在α-碳金属化并用相应的烷基卤化物进行捕集实验后,获得了C取代的双(三乙氧基甲硅烷基)甲烷。如果是三(三乙氧基甲硅烷基)氨基甲酸酯,则只有MeI和Br 2能够提供预期的产品。出乎意料的是,CO 2插入,得到稳定烯酮,[(ETO)3的Si] 2 CCO。