SEMIPREPARATIVE SEPARATION OF MIXED SUBSTITUTED OCTA-(ORGANYLSILSESQUIOXANES) USING NORMAL-PHASE HPLC AND ITS SI-29 NMR SPECTROSCOPIC ANALYSIS

被引:40
作者
HENDAN, BJ [1 ]
MARSMANN, HC [1 ]
机构
[1] UNIV GESAMTHSCH PADERBORN,FACHBEREICH CHEM & CHEM TECH,WARBURGER STR 100,D-33098 PADERBORN,GERMANY
关键词
D O I
10.1016/0022-328X(94)87144-2
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Cohydrolysis of organotrichloro or organotrimethoxy silanes yields the mixed octa-(organosilsesquioxanes), (Si8O12)R8-nR(n)' (n = 0, 1, 2 (3 isomers); R = n-C3H7, R' = 3-ClC3H6 (I), 3-HSC3H6 (III), C3H5 (IV) and R = C2H5, R' = C2H3 (V)); they can be separated by normal phase HPLC. The degree of substitution and the substitution pattern can be recognized by the distribution of Si-29-NMR signals, where a linear dependence of the chemical shift of the R substituted silicon atoms on the number of R' substituted neighbours is observed.
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收藏
页码:33 / 38
页数:6
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