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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Synthesis and structural characterization of 20-membered macrocyclic rings bearing trans-chelating bis(N-heterocyclic carbene) ligands and the catalytic activity of their palladium(ii) complexes
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Synthesis and structural characterization of 20-membered macrocyclic rings bearing trans-chelating bis(N-heterocyclic carbene) ligands and the catalytic activity of their palladium(ii) complexes

机译：携带反式螯合双（N-杂环碳烯）配体及其钯（II）复合物的催化活性的20元大环环的合成和结构表征

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摘要

Macrocycles consisting of a 20-membered ring containing two imidazolium salt functionalities and of the formula [PhCH2N(CH2CH2CH2)Im(CH2CH2CH2)(2)][Br](2) (Im = imidazole = 3a, benzimidazole = 3b) were synthesized in 70-75% yields. These salts serve as precursors to macrocycles containing two N-heterocyclic carbene (NHC) moieties. Reaction of the macrocyclic salts 3a and 3b with silver oxide afforded macrocyclic-bis(NHC)silver(i) complexes 4a and 4b. Single-crystal X-ray diffraction studies of macrocyclic-bis(NHC)silver(i) complex 4a revealed a tetranuclear silver core with a short Ag-Ag distance (2.9328 angstrom). Complexes 4a and 4b serve as carbene transfer reagents to Pd. The treatment of macrocyclic-bis(NHC)silver(i) complexes 4a and 4b with one equivalent of PdCl2(MeCN)(2) in methylene chloride afforded square-planar trans-macrocyclic-bis(NHC)Pd(ii)X-2 complexes 5a and 5b. Preliminary screening of these palladium complexes showed they are competent precatalysts for Heck and Suzuki coupling reactions.
机译：由含有两个咪唑鎓盐官能度的20元环的及下式的大环化合物[PhCH2N（CH2CH2CH2）IM（CH2CH2CH2）（2）] [BR]（2）（IM =咪唑= 3A，苯并咪唑= 3B）是在合成70-75％的产量。这些盐作为前体含有两个N-杂环卡宾（NHC）部分的大环。大环的盐3a和3b与氧化银，得到大环双（NHC）银（I）络合物4a和4b的反应。大环双（NHC）银（I）的单晶X射线衍射研究复杂的图4a揭示了具有短的Ag-的Ag距离（2.9328埃）四核银核。配合物4A和4B作为卡宾转移剂以Pd等。大环双治疗（NHC）银（I）配合物4a和4b与一个当量的PdCl 2（MeCN中）（2）在二氯甲烷中，得到正方形平面的反式大环双（NHC）的Pd（II）X-2复合物5A和5B。这些钯复合物的初步筛选结果显示他们对Heck和铃木偶联反应能力的预催化剂。

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