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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Electron-rich, bulky PNN-type ruthenium complexes: synthesis, characterization and catalysis of alcohol dehydrogenation
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Electron-rich, bulky PNN-type ruthenium complexes: synthesis, characterization and catalysis of alcohol dehydrogenation

机译：富电子的大体积PNN型钌配合物：醇脱氢的合成，表征和催化

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摘要

Reaction of the electron-rich, bulky tridentate PNN ligand (PNN = 2-di-tert-butylphosphinomethyl-6-diethylaminomethylpyridine) with Ru(PPh3)(3)Cl-2 at 65 degrees C resulted in formation of the mononuclear dinitrogen complex (PNN)Ru(Cl)(2)N-2 1a (minor) and the N-2 bridged Ru(II) dinuclear complex [(PNN)Ru(Cl)(2)](2)(mu-N-2) 1b (major). These complexes can be interconverted; passing argon through a solution of the mixture resulted in formation of pure 1b. The cationic square-pyramidal [(PNN)Ru(PPh3)Cl]OTf 2 was obtained by the reaction of complex 1b with silver triflate followed by PPh3. Reaction of complex 1b with CO yielded (PNN)Ru(CO)Cl-2 3, which upon reaction with one equiv. of AgBF4 gave the cationic [(PNN)Ru(CO)Cl]BF4 4. The dicationic [(PNN)Ru(CO)(H2O)(acetone)](BF4)(2) 5 was obtained from 3 with 2 equiv. of AgBF4 in acetone solution. Complexes 1b, 2 and 5 were structurally characterized by X-ray crystallography. Complexes 1b and 3, upon addition of an equivalent of base, catalyzed the dehydrogenation of secondary alcohols to the corresponding ketones and primary alcohols to esters in good yields and high selectivity accompanied with the evolution of hydrogen gas.
机译：富电子的大体积三齿PNN配体（PNN = 2-二叔丁基膦甲基-6-二乙基氨基甲基吡啶）与Ru（PPh3）（3）Cl-2在65°C下反应导致单核二氮配合物（ PNN）Ru（Cl）（2）N-2 1a（次要）和N-2桥接的Ru（II）双核复合物[（PNN）Ru（Cl）（2）]（2）（mu-N-2） 1b（主要）。这些复合体可以互换。使氩气通过混合物的溶液导致形成纯的1b。通过配合物1b与三氟甲磺酸银，然后与PPh3的反应，获得阳离子方形金字塔形的[（PNN）Ru（PPh3）Cl] OTf 2。配合物1b与CO反应生成（PNN）Ru（CO）Cl-2 3，当与1当量反应时。 AgBF 4的合成得到阳离子的[（PNN）Ru（CO）Cl] BF 44。由3当量为2当量获得了二价的[（PNN）Ru（CO）（H 2 O）（丙酮）]（BF 4）（2）5。在丙酮溶液中的AgBF 4。配合物1b，2和5在结构上通过X射线晶体学表征。在加入等价的碱后，配合物1b和3催化仲醇脱氢为相应的酮，伯醇为酯的脱氢反应，收率高，选择性高，伴随有氢气的析出。

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