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Syntheses, structures, and immobilization of ruthenium(II) complexes with alkoxysilane groups functionalized N,N′-diamine and phosphine ligands
Journal of Coordination Chemistry ( IF 1.9 ) Pub Date : 2020-04-17 , DOI: 10.1080/00958972.2020.1763969
Jiao Ji 1 , Li-Miao Shi 1 , Fule Wu 1 , Zhi-Feng Xin 1 , Ai-Quan Jia 1 , Qian-Feng Zhang 1
Affiliation  

Abstract Treatment of [RuCl2(PPh3)3] with N-(β-aminoethyl)-γ-aminopropylmethylbimethoxysilane (L1) in tetrahydrofuran at room temperature gave a mononuclear ruthenium(II) complex [Ru(PPh3)2Cl2 (κ2-N,N-L1)] (1). Condensation of γ-aminopropyltriethoxysilane and potassium diphenylphosphine in the molar ratio of 1:1 in tetrahydrofuran afforded phosphine (PPh2)(CH2)3Si(OEt)3 (L2) with ethoxysilane groups. Reaction of [Ru(η6-p-cymene)Cl2]2 with L2 in refluxing tetrahydrofuran afforded a ruthenium(II) phosphine complex [Ru(η6-p-cymene)Cl2(κ-P-L2)] (2). Complexes 1 and 2 were systematically characterized by microanalyses, FT-IR, and NMR spectroscopies. Their structures have been unambiguously established by single-crystal X-ray diffraction. Immobilization of 1 and 2 on SBA-15 and characterization of these hybrid heterogeneous catalysts were studied by transmission electron microscopy (TEM), FT-IR, and low-pressure N2 adsorption/desorption measurements. Transfer hydrogenation of acetophenone was also briefly investigated with the heterogeneous catalysts. Graphical Abstract

中文翻译:

具有烷氧基硅烷基团官能化 N,N'-二胺和膦配体的钌 (II) 配合物的合成、结构和固定

摘要 在室温下在四氢呋喃中用 N-(β-氨基乙基)-γ-氨基丙基甲基二甲氧基硅烷 (L1) 处理 [RuCl2(PPh3)3] 得到单核钌 (II) 配合物 [Ru(PPh3)2Cl2 (κ​​2-N,N -L1)] (1)。γ-氨基丙基三乙氧基硅烷和二苯基膦钾在四氢呋喃中以 1:1 的摩尔比缩合得到带有乙氧基硅烷基团的膦 (PPh2)(CH2)3Si(OEt)3 (L2)。[Ru(η6-p-cymene)Cl2]2 与 L2 在回流的四氢呋喃中反应得到钌 (II) 膦配合物 [Ru(η6-p-cymene)Cl2(κ-P-L2)] (2)。配合物 1 和 2 通过微量分析、FT-IR 和 NMR 光谱系统地表征。它们的结构已通过单晶 X 射线衍射明确确定。通过透射电子显微镜 (TEM)、FT-IR 和低压 N2 吸附/解吸测量研究了 1 和 2 在 SBA-15 上的固定和这些混合多相催化剂的表征。苯乙酮的转移氢化也用非均相催化剂进行了简要研究。图形概要
更新日期:2020-04-17
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