Bildung siliciumorganischer Verbindungen. 102. Zur Umsetzung von Chlormethanen mit elementarem Silicium (Bildung und Aufklärung linearer Carbosilane) |
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Authors: | G. Fritz,A. W rsching |
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Affiliation: | G. Fritz,A. Wörsching |
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Abstract: | Formation of Organosilicon Compounds. 102. Reaction of Chlormethanes with Elemental Silicon. (Formation and Investigation of Linear Carbosilanes) Reactions of CH2Cl2, HCCl3 and CCl4 with silicon (Cu catalyst) in a fluid bed at about 320°C were carried out to investigate especially the Si-rich compounds. In the reactions of CH2Cl2 and CHCl3, but not of CCl4, in addition to already published compounds Si-rich viscous products are formed. The SiCl-containing mixtures were reacted with LiAlH4, and the SiH-containing derivatives were separated by means of HPLC. CH2Cl2/Si forms unbranched chains of carbosilanes as SinCn–1H4n (n = 4—12,2 terminal SiH3 groups) and SinCnH4n+2 (n = 4—9, 1 terminal SiH3 and 1 CH3 group) as well as 1,3,5-trisilacyclohexanes with carbosilane chains of various length attached either to a Si atom or to a C atom. CHCl3/Si yields in addition to unbranched chains with terminal silyl group chains with one or two C-branches and 1,3,5-trisilacyclohexanes with 1, 2, or 3 silyl substituents attached to C atoms. The structure of the isolated compounds was investigated by nmr and mass spectrometry. |
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