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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 21, Number 10
BKCSDE 21(10)
October 20, 2000 

Synthesis of Tris(silyl)methanes by Modified Direct Process
Chang Yeob Lee, Joon Soo Han, Hyung Sic oh, Bok RyuI Yoo, Il Nam Jung
Direct reaction of elemental silicon with a mixture of (dichloromethyl)silanes 1 [Cl₃-nMenSiCHCl₂: n = 0 (a), n = 1(b), n = 2(c), n = 3(d)] and hydrogen chloride has been studied in the presence of copper catalyst using a stirred bed reactor equipped with a spiral band agitator at various temperatures from 240℃ to 340℃. Tris(si-lyl) methanes with Si-H bonds, 3a-d [Cl₃-nMenSiCH(SiHCl₂)₂], and 4a-d [Cl₃-nMenSiCH(SiHCl₂)(SiCl₃)], were obtained as the major products and tris(silyl)methanes having no Si-H bond, 5a-d [Cl₃-nMenSiCH(SiCl₃)₂], as the minor product along with byproducts of bis(chlorosilyl)methanes, derived from the reaction of silicon with chloromethylsilane formed by the decomposition of 1. In addition to those products, trichlorosilane and tetra-chlorosilane were produced by the reaction of elemental silicon with hydrogen chloride. The decomposition of 1 was suppressed and the production of polymeric carbosilanes reduced by adding hydrogen chloride to 1. Cad-mium was a good promoter for and the optimum temperature for this direct synthesis was 280℃.
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