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一种新型功能化介孔基质负载 Pd(II)-席夫碱配合物:Suzuki-Miyaura 偶联反应的高效催化剂。

A new functionalized mesoporous matrix supported Pd(II)-Schiff base complex: an efficient catalyst for the Suzuki-Miyaura coupling reaction.

机构信息

Department of Chemistry, Sambhu Nath College, Labpur, Birbhum, 731303, West Bengal, India.

出版信息

Dalton Trans. 2010 Jul 28;39(28):6395-402. doi: 10.1039/c003142a. Epub 2010 Jun 7.

Abstract

A new Pd(II) bounded 2D-hexagonally ordered functionalized MCM-41 type material (IV) has been synthesized. Functionalization was carried out by the anchoring of 3-aminopropyltriethoxysilane in the MCM-41 type mesoporous material, followed by grafting with 2,6-diacetylpyridine (DAP) to give a N3-type Schiff base chelating attachment for the Pd(II) species. Fourier transform infrared (FTIR), powder X-ray diffraction (PXRD) and high resolution transmission electron microscopy (HRTEM) studies have been used to characterize the material. Material IV behaves as a highly active catalyst towards Suzuki-Miyaura cross-coupling reaction for the synthesis of biaryl organics. In addition, IV acts as a true heterogeneous catalyst in coupling reaction. It was found that this catalyst is highly efficient and recyclable towards Suzuki-Miyaura reaction with high turn over frequencies. X-Ray photoelectron spectroscopic (XPS) analysis was employed to understand the oxidation state of the palladium atom in the catalyst (IV) and its loading in the material.

摘要

一种新的 Pd(II) 配位的二维六边形有序功能化 MCM-41 型材料 (IV) 已被合成。功能化是通过在 MCM-41 型介孔材料中锚定 3-氨丙基三乙氧基硅烷,然后接枝 2,6-二乙酰基吡啶 (DAP) 来实现的,从而得到 N3 型席夫碱螯合配体,用于 Pd(II) 物种。傅里叶变换红外 (FTIR)、粉末 X 射线衍射 (PXRD) 和高分辨率透射电子显微镜 (HRTEM) 研究用于表征该材料。材料 IV 对 Suzuki-Miyaura 交叉偶联反应合成联芳有机物具有很高的活性。此外,IV 在偶联反应中充当真正的多相催化剂。研究发现,该催化剂对 Suzuki-Miyaura 反应具有高效和可回收性,具有高的周转频率。X 射线光电子能谱 (XPS) 分析用于了解催化剂 (IV) 中钯原子的氧化态及其在材料中的负载量。

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