磁化SBA-15负载双(肟)钯环作为Mizoroki-Heck反应的高效可回收催化剂

IF 2.1 4区 化学 Q3 CHEMISTRY, PHYSICAL Catalysis Surveys from Asia Pub Date : 2023-04-28 DOI:10.1007/s10563-023-09396-w
Fatemeh Ghahramani, Yagoub Mansoori, Abolfazl Bezaatpour, Dolores Esquivel, M. Angeles Navarro
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引用次数: 0

摘要

在此,我们报道了在磁性介孔二氧化硅(Fe3O4@SBA-15)上锚定双(肟钯环)加合物。磁性介孔二氧化硅依次用(3-氨基丙基)三乙氧基硅烷(APTES)、三聚氰尿酸(CC)和4-羟基苯乙酮肟衍生的钯环处理得到Fe3O4@SBA-AP-CC-bis(肟钯环)。采用FT-IR、CP MAS 13C NMR、扫描电镜(SEM)、振动样品磁强计(VSM)、brunauer - emmet - teller表面积测量(SBET)和x射线衍射光谱(XRD)对所制得的纳米催化剂进行了表征。X射线光电子能谱(XPS)证实了钯的(+ 2)氧化值。研究了Fe3O4@SBA-AP-CC-bis(肟palladacycle)在Mizoroki-Heck反应中的催化潜力。考察了溶剂、碱、温度、钯含量等不同反应条件对反应性能的影响。n -甲基吡咯烷酮(NMP)溶剂、0.5 mol%的pd -催化剂、NaOAc碱、120℃的反应温度为Heck交叉偶联反应提供了最佳条件。在Mizoroki-Heck反应中,该催化剂显示出广泛的底物范围,包括芳基卤化物(I, Br, Cl)和烯烃,使用低催化剂负载(Pd 0.09 mol%)。其(肟palladacycle)具有易于磁分离,稳定性和可回收性超过五次运行。
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Bis(Oxime Palladacycle) Supported on Magnetized SBA-15 as an Efficient and Retriveble Catalyst for the Mizoroki–Heck Reaction

Herein, we report the anchoring of a bis(oxime palladacycle) adduct on magnetic mesoporous silica (Fe3O4@SBA-15). Magnetic mesoporous silica was successively treated with (3-aminopropyl) triethoxysilane (APTES), cyanuric chloride (CC), and 4-hydroxyacetophenone oxime-derived palladacycle to give Fe3O4@SBA-AP-CC-bis(oxime palladacycle). The obtained nano-catalyst was characterized by FT-IR spectroscopy, CP MAS 13C NMR spectroscopy, scanning electron microscopy (SEM), vibrating sample magnetometry (VSM), Brunauer–Emmett–Teller surface area measurement (SBET) and X-ray diffraction spectroscopy (XRD). X‐Ray photoelectron spectroscopy (XPS) corroborated the (+ 2) oxidation number for palladium. The catalytic potential of Fe3O4@SBA-AP-CC-bis(oxime palladacycle) was explored in the Mizoroki–Heck reaction. The effects of different reaction conditions, including the solvent, the base, temperature, and palladium content, were studied in detail. The N-methylpyrrolidone (NMP) solvent, 0.5 mol% of the Pd-catalyst, the NaOAc base, and the reaction temperature of 120 °C, provided the best conditions for the Heck cross-coupling reaction. The catalyst showed a wide substrate scope, including aryl halides (I, Br, Cl) and olefins, in the Mizoroki–Heck reaction, using low catalyst loadings viz., Pd 0.09 mol%. The bis(oxime palladacycle) enjoys easy magnetic separation, stability, and recyclability over five runs.

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来源期刊
Catalysis Surveys from Asia
Catalysis Surveys from Asia 化学-物理化学
CiteScore
4.80
自引率
0.00%
发文量
29
审稿时长
>12 weeks
期刊介绍: Early dissemination of important findings from Asia which may lead to new concepts in catalyst design is the main aim of this journal. Rapid, invited, short reviews and perspectives from academia and industry will constitute the major part of Catalysis Surveys from Asia . Surveys of recent progress and activities in catalytic science and technology and related areas in Asia will be covered regularly as well. We would appreciate critical comments from colleagues throughout the world about articles in Catalysis Surveys from Asia . If requested and thought appropriate, the comments will be included in the journal. We will be very happy if this journal stimulates global communication between scientists and engineers in the world of catalysis.
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