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Ultra-small palladium nano-particles synthesized using bulky S/Se and N donor ligands as a stabilizer: application as catalysts for Suzuki–Miyaura coupling

机译:使用庞大的S / Se和N供体配体作为稳定剂合成的超小钯纳米粒子:作为Suzuki-Miyaura偶联催化剂的应用

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Two chalcogenated ligands L1 and L2 containing anthracene core and amine functionality have been synthesized. Both the ligands have been characterized using ~(1) H and ~(13) C{ ~(1) H} NMR techniques. The structure of L1 has also been corroborated by single crystal X-ray diffraction. Application of L1 and L2 as stabilizers for palladium nano-particles (NPs) has been explored and six different types of NPs 1–6 have been prepared by varying the quantity of stabilizer. The nano-particles have been characterized by PXRD, EDX, and HRTEM techniques. The size of NPs has been found to be in the range of ~1–2 nm, 2–3 nm, 4–6 nm, 1–2 nm, 1–2 nm and 3–5 nm for 1–6 respectively. The catalytic activities of 1–6 have been explored for Suzuki–Miyaura coupling of phenyl boronic acid with various aryl halides. These NPs showed good catalytic activity for various aryl chlorides/bromides at low catalyst loading (5 mg). Among 1–6 , the highest activity has been observed for NPs 1 , probably due to their relatively small size and high uniformity in the dispersion. The recyclability of the NPs upto 5 catalytic cycles is a distinct advantage.
机译:已经合成了两个含蒽核心和胺官能团的硫族配体L1和L2。两种配体均已使用〜(1)H和〜(13)C {〜(1)H} NMR技术进行了表征。 L1的结构也已通过单晶X射线衍射得到证实。研究了将L1和L2用作钯纳米颗粒(NPs)的稳定剂,并通过改变稳定剂的量制备了六种不同类型的NPs 1-6。纳米粒子已通过PXRD,EDX和HRTEM技术进行了表征。发现NP的大小分别在1-6 nm〜1-2 nm,2-3 nm,4-6 nm,1-2 nm,1-2 nm和3-5 nm范围内。苯并硼酸与各种芳基卤化物的Suzuki-Miyaura偶联已探索了1–6的催化活性。这些NP在低催化剂负载量(5 mg)下显示出对各种芳基氯化物/溴化物的良好催化活性。在1-6中,观察到最高的NPs 1活性,可能是由于它们的尺寸相对较小且分散均匀性很高。 NPs的可回收性高达5个催化循环是一个明显的优势。

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