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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Ti and Zr bidentate bis-phosphinimide complexes
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Ti and Zr bidentate bis-phosphinimide complexes

机译：Ti和Zr双齿双膦亚酰亚胺配合物

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摘要

The diphosphines m-C_6H_4(CH_2Pt-Bu_2)_2 1 and m-C_6H_4(CH_2PCy_2)_2 were prepared and oxidized with Me_3SiN_3 to m-C_6H_4(CH_2(t-Bu_2)PNSiMe_3)_2 3 and m-C_6H_4(CH_2(Cy_2)PNSiMe_3)_2 4, and subsequently converted to m-C_6H_4(CH_2(t-Bu_2)PNH)_2 5 and m-C_6H_4(CH_2(Cy)_2PNH)_2 6. Reaction of 5 and 6 with Ti(NMe_2)_4 afforded the yellow compounds m-C_6H_4(CH_2(t-Bu_2)PN)_2Ti(NMe_2)_2 7 and m-C_6H_4(CH_2(Cy)_2PN)_2Ti(NMe_2)_2 8, and the low abundance by-product m-C_6H_4(CH_2(t-Bu_2)PN)_2TiBr(NMe_2) 9. In a similar manner, the species m-C_6H_4(CH_2(t-Bu_2)PN)_2Zr(NEt_2)_2 10 was prepared from Zr(NEt_2)_4. Compounds 8, 9 and 10 were converted to C_6H_4(CH_2(t-Bu_2)PN)_2TiBr_2 11, m-C_6H_4(CH_2(Cy)_2PN)_2TiCl_2 13 and C_6H_4(CH_2(t-Bu_2)PN)_2ZrCl_2 14 via reaction with Me_3SiX (X = Br, Cl). Alternatively, m-C_6H_4(CH_2(t-Bu_2)PN)_2TiCl_2 12 and 13 were prepared in low yield from reaction of 3 or 4 with TiCl_4. Alkylation of 11 with MeMgBr and PhCH_2MgBr proceeded to give m-C_6H_4(CH_2(t-Bu_2)PN)_2TiMe_2 15 and m-C_6H_4(CH_2(t-Bu_2)PN)_2Ti(CH_2Ph)_2 16 respectively. The species (m-C_6H_4(CH_2(t-Bu_2)PN)_2)_2Zr 17 was prepared from Zr(CH_2Ph)_4. These synthetic routes are described and the implications for applications in olefin polymerization catalysis are considered. X-Ray structural data for compounds 1, 3, 4, 5, 8, 9 and 16 are reported.
机译：制备二膦m-C_6H_4（CH_2Pt-Bu_2）_2 1和m-C_6H_4（CH_2PCy_2）_2并用Me_3SiN_3氧化为m-C_6H_4（CH_2（t-Bu_2）PNSiMe_3）_2 3和m-C_6H_4（CH_2（C_2） PNSiMe_3）_2 4，然后转化为m-C_6H_4（CH_2（t-Bu_2）PNH）_2 5和m-C_6H_4（CH_2（Cy）_2PNH）_26。5和6与Ti（NMe_2）_4反应得到黄色化合物m-C_6H_4（CH_2（t-Bu_2）PN）_2Ti（NMe_2）_2 7和m-C_6H_4（CH_2（Cy）_2PN）_2Ti（NMe_2）_2 8和低丰度副产物m-C_6H_4（CH_2） （t-Bu_2）PN）_2TiBr（NMe_2）9.以类似的方式，从Zr（NEt_2）_4制备出m-C_6H_4（CH_2（t-Bu_2）PN）_2Zr（NEt_2）_2 10。化合物8、9和10通过与C_6H_4（CH_2（t-Bu_2）PN）_2TiBr_2 11，m-C_6H_4（CH_2（Cy）_2PN）_2TiCl_2 13和C_6H_4（CH_2（t-Bu_2）PN）_2ZrCl_2 14转化为C_6H_4 Me_3SiX（X = Br，Cl）。或者，通过3或4与TiCl_4的反应以低收率制备m-C_6H_4（CH_2（t-Bu_2）PN）_2TiCl_2 12和13。将11与MeMgBr和PhCH_2MgBr烷基化分别得到m-C_6H_4（CH_2（t-Bu_2）PN）_2TiMe_2 15和m-C_6H_4（CH_2（t-Bu_2）PN）_2Ti（CH_2Ph）_2 16。由Zr（CH_2Ph）_4制备了（m-C_6H_4（CH_2（t-Bu_2）PN）_2）_2Zr 17物种。描述了这些合成路线，并考虑了其在烯烃聚合催化中的应用意义。报告了化合物1、3、4、5、8、9和16的X射线结构数据。

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