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首页> 外文期刊>RSC Advances >Synthesis of a recyclable and efficient Pd(II) 4-(2-pyridyl)-1,2,3-triazole complex over a solid periodic mesoporous organosilica support by 'click reactions' for the Stille coupling reaction
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Synthesis of a recyclable and efficient Pd(II) 4-(2-pyridyl)-1,2,3-triazole complex over a solid periodic mesoporous organosilica support by 'click reactions' for the Stille coupling reaction

机译：通过Stiller偶联反应的“点击反应”，在固体周期性介孔有机硅载体上合成可回收且有效的Pd（II）4-（2-吡啶基）-1,2,3-三唑配合物

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摘要

A highly efficient, reusable B-PMO-TZ-Pd(II) catalyst was synthesized by anchoring 4-(2-pyridyl)-4-(2-pyridyl)-1,2,3-triazole ligand over the surface of an organo-functionalized benzene support containing periodic mesoporous organosilica (B-PMO) via "click reaction" and the subsequent complexation with PdCl2. B-PMO materials with uniform hexagonal arrangements were prepared using C-16 alkyl trimethyl ammonium bromide [CTAB] surfactant under basic conditions. The physiochemical properties of the functionalised catalyst were analysed by elemental analysis, ICP-OES, XRD, N-2 sorption, TGA & DTA, solid state C-13, Si-29 NMR spectra, FT-IR, XPS, UV-vis, SEM and TEM. XRD and N-2 sorption revealed the morphological and textural properties of the synthesized catalyst, confirming that ordered mesoporous channel structure was retained even after the multistep synthetic procedure. The (100), (110) and (200) reflections in B-PMO are evidence of its good structural stability and the existence of long range order. The TGA-DTA results reveal that the synthesized catalyst B-PMO-TZ-Pd(II) was thermally stable, even at high temperature. The organic moieties anchored over the surface of B-PMO were demonstrated by solid state C-13 NMR and FT-IR spectroscopy. Solid state Si-29 NMR spectroscopy provides information about the degree of functionalization of the surface silanol group. The electronic environment and oxidation state of Pd in B-PMO-TZ-Pd(II) were monitored by XPS and UV-visible techniques. Moreover, the morphologies and topographic information of the synthesized B-PMO-TZ-Pd(II) catalyst were confirmed by SEM and TEM analyses. The catalytic properties of the catalyst for the Stille coupling reaction were screened, and higher catalytic activities with high TONs were observed. The anchored solid B-PMO-TZ-Pd(II) catalyst can be recycled efficiently and reused several (four) times without a major loss in reactivity.
机译：通过将4-（2-吡啶基）-4-（2-吡啶基）-1,2,3-三唑配体锚固在有机表面上来合成高效，可重复使用的B-PMO-TZ-Pd（II）催化剂-功能化的苯载体，通过“点击反应”以及随后与PdCl2的络合，含有周期性的介孔有机硅（B-PMO）。在碱性条件下，使用C-16烷基三甲基溴化铵[CTAB]表面活性剂制备具有均匀六边形排列的B-PMO材料。通过元素分析，ICP-OES，XRD，N-2吸附，TGA和DTA，固态C-13，Si-29 NMR光谱，FT-IR，XPS，UV-vis， SEM和TEM。 XRD和N-2吸附揭示了合成催化剂的形态和织构性质，证实了即使经过多步合成程序，也保留了有序的中孔通道结构。 B-PMO中的（100），（110）和（200）反射证明了其良好的结构稳定性和远距离有序性。 TGA-DTA结果表明，即使在高温下，合成的催化剂B-PMO-TZ-Pd（II）也是热稳定的。通过固态C-13 NMR和FT-IR光谱证实了锚定在B-PMO表面的有机部分。固态Si-29 NMR光谱学提供了有关表面硅烷醇基官能化程度的信息。通过XPS和紫外可见技术监测B-PMO-TZ-Pd（II）中Pd的电子环境和氧化态。此外，通过SEM和TEM分析证实了合成的B-PMO-TZ-Pd（II）催化剂的形貌和形貌信息。筛选了用于Stille偶联反应的催化剂的催化性能，并观察到在高TON下具有更高的催化活性。锚固的固体B-PMO-TZ-Pd（II）催化剂可以有效地循环利用并重复使用几（四）次，而不会显着降低反应活性。

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