Department of Chemistry, Sambhu Nath College, Labpur, Birbhum, 731303, West Bengal, India.
Dalton Trans. 2010 Jul 28;39(28):6395-402. doi: 10.1039/c003142a. Epub 2010 Jun 7.
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.
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。