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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Palladium(II) complexes of N, N-diphenylacetamide based thio/selenoethers and flower shaped Pd16S7 and prismatic Pd17Se15 nano-particles tailored as catalysts for C-C and C-O coupling
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Palladium(II) complexes of N, N-diphenylacetamide based thio/selenoethers and flower shaped Pd16S7 and prismatic Pd17Se15 nano-particles tailored as catalysts for C-C and C-O coupling

机译：基于N，N-二苯基乙酰胺的硫代/硒的钯/硒络合物和花形PD16S7和棱镜PD17SE15纳米颗粒作为C-C和C-O耦合的催化剂定制

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2-Bromo-N, N-diphenylacetamide (P1) prepared by reacting diphenylamine with a-bromoacetyl bromide, on treatment with Na2S and Na2Se generated in situ, has resulted in thio and selenoether ligands, L1 ((Ph2NCOCH2)(2)S) and L2 ((Ph2NCOCH2)(2)Se), respectively. Reacting these ligands with Na2PdCl4 in ethanol at room temperature resulted in their complexes [Pd(L1/L2)(2)Cl-2] (C1/C2). P1, L1, L2, C1 and C2 were characterized by H-1, C-13{1H} and Se-77{H-1} NMR spectroscopy, IR spectroscopy and High resolution mass spectrometry (HR-MS). Single crystal structures of all the five compounds were determined by X-ray diffraction. In both C1 and C2 the geometry of Pd is nearly square planar. Flower shaped Pd16S7 (size 26-50 nm) and prismatic Pd17Se15 NPs (size 20-55 nm) were synthesized by a single source precursor route (thermolysis at similar to 280 degrees C in trioctylphosphine) from air and moisture insensitive C1 and C2, respectively. These shapes of the two nanophases were unknown hitherto. They were characterized by powder X-ray diffraction (PXRD), SEM-EDX and HR-TEM and found to show good catalytic activity for SuzukiMiyaura (Pd loading 0.5 mol%; yield up to 96%) and C-O (Pd loading 0.5 mol%; yield up to 96%) coupling reactions (at 100 degrees C) of aryl bromides with phenylboronic acid and phenol, respectively. The complexes C1 and C2 were found very efficient for Suzuki-Miyaura and C-O coupling as revealed by their optimum loading of 0.0001-0.01 and 0.1 mol% of Pd, respectively, for the two reactions. The reuse of the complexes or NPs as a catalyst is demonstrated.
机译：通过与硫化钠和Na2Se治疗原位产生的二苯胺与溴乙酰溴反应，制备2-溴-N，N-二苯基乙酰胺（P1），已经导致硫基和硒醚配体，L1（（Ph2NCOCH2）（2）S）和L2（（Ph2NCOCH2）（2）Se）中，分别。在室温下在乙醇反应这些配体与Na2PdCl4导致其在配合物[钯（L1 / L2）（2）CL-2]（C1 / C2）。由H-1，C-13 C {1 H}和Se-77 {H-1} NMR光谱，IR光谱和高分辨率质谱（HR-MS）P1，L1，L2，C1和C2进行了表征。所有五种化合物的单晶结构经X射线衍射确定。在C1和C2的Pd的几何形状几乎是正方形的平面。花形Pd16S7（尺寸26-50纳米）和棱柱Pd17Se15的NP（20-55大小纳米）由单个前体源路径从空气和水分不敏感分别C1和C2，（以类似于280摄氏度在三辛基膦热分解）的合成。两个纳米相的这些形状不明至今。 CO（Pd负载量为0.5mol％和;它们是由粉末X射线衍射（PXRD），SEM-EDX和HR-TEM表征和发现显示良好的催化活性为SuzukiMiyaura（收率高达96％Pd载量0.5摩尔％） ;收率高达96％）偶联反应分别与苯基硼酸和苯酚，芳基溴化物的（在100℃）。配合物C1和C2被发现非常有效的铃木 - 宫浦和C-O耦合通过0.0001-0.01和0.1摩尔％的Pd，分别的它们的最佳装载所揭示，对于两个反应。的配合物或纳米颗粒作为催化剂的重复使用是证明。

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