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Alkylruthenium Complexes Containing Polypyridyl Ligands: Synthesis, Characterization, and Immobilization on Silica

Authors Huang, Enrique Kwan HKUST affiliated (currently or previously)
Cheung, Wai-Man HKUST affiliated (currently or previously)
Chan, Ka-Wang HKUST affiliated (currently or previously)
Lam, Frank Leung-Yuk HKUST affiliated (currently or previously)
Hu, Xijun View this author's profile
Zhang, Qian-Feng HKUST affiliated (currently or previously)
Williams, Ian Duncan View this author's profile
Leung, Wa-Hung View this author's profile
Issue Date 2013
Source European Journal of Inorganic Chemistry , (16), June 2013, p. 2893-2899
Summary The treatment of [Ru(CO)2Cl2]x with 4,4,4-tri-tert-butyl-2,2:6,6-terpyridyl (tbtpy) in tetrahydrofuran at reflux afforded trans-[Ru(tbtpy)Cl2(CO)] (1). The alkylation of complex 1 with excess Me3SiCH2MgCl afforded a mixture of trans-[Ru(tbtpy)(CH2SiMe3)2(CO)] (2) and trans-[Ru(tbtpy)(CH2SiMe3)Cl(CO)] (3), whereas complex 3 could be obtained in good yield by the alkylation of complex 1 with 1 equiv. of Me3SiCH2MgCl. On the other hand, the alkylation of 1 with MeLi and PhCH2MgBr afforded the monoalkyl complexes [Ru(tbtpy)(Me)Cl(CO)] (4) and [Ru(tbtpy)(CH2Ph)Cl0.5Br0.5(CO)] (5), respectively. The crystal structure of complex 5 was determined. Complex 2 and the previously prepared mer-[Ru(dtbpy)(CH2SiMe3)3(NO)] (dtbpy = 4,4-di-tert-butyl-2,2-bipyridyl) were immobilized on SBA-15 by treating the Ru complexes with SBA-15 in benzene at room temperature. 1H NMR spectroscopy indicated that the reaction of complex 2 and [Ru(dtbpy)(CH2SiMe3)3(NO)] with SBA-15 in C6D6 resulted in the formation of approximately 1 equiv. of SiMe4, which suggests the grafted species are possibly (SiO)Ru(tbtpy)(CH2SiMe3)(CO) and (SiO)Ru(dtbpy)(CH2SiMe3)2(NO), respectively. The Ru-grafted SBA-15 materials were characterized by IR, reflectance UV/Vis, and X-ray photoelectron spectroscopy as well as transmission electronic microscopy, and their catalytic performance in the oxidation of benzyl alcohol with tert-butyl hydroperoxide was examined.
ISSN 1434-1948
Language English
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