Synthesis of a [(π-Cyano-nacnac)Cp]zirconium complex and its remote activation for ethylene polymerization

Cabrera A.R.; Schneider Y.; Valderrama M.; Fr?hlich R.; Kehr G.; Erker G.; Rojas R.S.

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Synthesis of a [(π-Cyano-nacnac)Cp]zirconium complex and its remote activation for ethylene polymerization

机译：[（π-Cyano-nacnac）Cp]锆配合物的合成及其对乙烯聚合的远程活化

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The NC-nacnacH ligand (2) was prepared by the deprotonation of the unsymmetrically N5-phenyl, N1-2,6-diisopropylphenyl substituted bis(imino) acetylacetonate nacnacH system (1) with n-butyllithium followed by cyanation with tosyl cyanide. Subsequent deprotonation (KH) gave the [NC-nacnac]K salt (3), which was transmetalated by reacting it with CpZrCl_3(dme), to yield the complex (NC-nacnac)CpZrCl_2 (5). Addition of one molar equivalent of B(C_6F_5)_3 gave [(C _6F_5)_3B-NC-nacnac]CpZrCl_2 (6). The compounds 2, 5, and 6 were characterized by X-ray diffraction. Activation of 5 with MAO gave an active homogeneous Ziegler-Natta catalyst for ethylene polymerization. The (NC-nacnac)CpZrCl_2/MAO system is ca. 7 times more active than the CN-free reference system (nacnac)CpZrCl_2 (4)/MAO. The B(C_6F_5)_3-containing system 6/MAO has an activity similar to 5/MAO but allows for much lower MAO concentration before the catalytic activity ceases.

机译：NC-nacnacH配体（2）的制备方法是，将不对称的N5-苯基，N1-2,6-二异丙基苯基取代的双（亚氨基）乙酰丙酮化nacnacH体系（1）用正丁基锂去质子化，然后用甲苯磺酰氰进行氰化。随后的去质子化（KH）得到[NC-nacnac] K盐（3），将其与CpZrCl_3（dme）反应进行金属转移，从而生成络合物（NC-nacnac）CpZrCl_2（5）。加入一摩尔当量的B（C_6F_5）_3，得到[（C_6F_5）_3B-NC-nacnac] CpZrCl_2（6）。化合物2、5和6通过X射线衍射表征。用MAO活化5得到用于乙烯聚合的活性均相齐格勒-纳塔催化剂。（NC-nacnac）CpZrCl_2 / MAO系统约为。活性是不含CN的参比系统（nacnac）CpZrCl_2（4）/ MAO的7倍。含B（C_6F_5）_3的系统6 / MAO具有与5 / MAO相似的活性，但在催化活性停止之前允许的MAO浓度低得多。

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《Organometallics》 |2010年第22期|共7页
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Cabrera A.R.; Schneider Y.; Valderrama M.; Fr?hlich R.; Kehr G.; Erker G.; Rojas R.S.;
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1. Synthesis of [(π-cyano-P-nacnac)Cp] and [(π-cyano-nacnac)Cp]- zirconium complexes, and their remote activation for ethylene polymerization [J] . Rojas R.S., Cabrera A.R., Peoples B.C., Dalton transactions: An international journal of inorganic chemistry . 2012,第4期

机译：[（π-氰基-P-nacnac）Cp]和[（π-氰基-P-nacnac）Cp]-锆配合物的合成及其对乙烯聚合的远程活化
2. Synthesis of a [(π-Cyano-nacnac)Cp]zirconium complex and its remote activation for ethylene polymerization [J] . Cabrera A.R., Schneider Y., Valderrama M., Organometallics . 2010,第22期

机译：[（π-Cyano-nacnac）Cp]锆配合物的合成及其对乙烯聚合的远程活化
3. Synthesis and characterization of materials prepared via the copolymerization of ethylene with 1-octadecene and norbornene using a [(π-cyano-nacnac)Cp] zirconium complex [J] . Cabrera A.R., Schneider Y., Valderrama M., Journal of Polymer Science, Part A. Polymer Chemistry . 2011,第7期

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4. Effect of Cyclopentadienyl Fragment in Polymerization of Ethylene, Propylene, and Styrene by Nonbridged Half-Metalloce Type Titanium and Zirconium Complexes of the Type, Cp'MCI_2 N(2,6-Me_2 C_6 H_3)(SiMe_3), -MAO Catalyst Systems [C] . Kotohiro NOMURA, Kensaku FUJII Tokyo Conference on Advanced Catalytic Science and Technology . 2003

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5. Chelating diamide complexes of titanium, zirconium and scandium: New polymerization catalysts based on non-Cp ligand environments. [D] . Scollard, John David. 1998

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Synthesis of a [(π-Cyano-nacnac)Cp]zirconium complex and its remote activation for ethylene polymerization

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