N,N-二甲基甲酰胺保护的钯纳米粒子的合成、表征及其在铃木-宫浦交叉偶联反应中的应用
Synthesis and Characterization of ,-Dimethylformamide-Protected Palladium Nanoparticles and Their Use in the Suzuki-Miyaura Cross-Coupling Reaction.
作者信息
Ishida Junya, Nakatsuji Masato, Nagata Tatsuki, Kawasaki Hideya, Suzuki Takeyuki, Obora Yasushi
机构信息
Department of Chemistry and Materials Engineering, Faculty of Chemistry, Materials, and Bioengineering, Kansai University, Suita, Osaka 564-8680, Japan.
The Institute of Scientific and Industrial Research, Osaka University, Mihogaoka, Ibaraki, Osaka 567-0047, Japan.
出版信息
ACS Omega. 2020 Apr 16;5(16):9598-9604. doi: 10.1021/acsomega.0c01006. eCollection 2020 Apr 28.
Herein, the synthesis of new ,-dimethylformamide (DMF)-protected palladium nanoparticles (Pd NPs-OAc) employing Pd (OAc) (= Pd(OCOCH)) as the NP precursor is reported. Pd NPs-OAc were comprehensively characterized by transmission electron microscopy, FT-IR, NMR, and X-ray photoelectron spectroscopy to determine the Pd NP size distribution and the coordination state of DMF. Pd NPs-OAc were compared with Pd NPs-Cl, using PdCl as the NP precursor. The Suzuki-Miyaura cross-coupling reaction proceeded efficiently in the presence of Pd NPs-OAc and a high catalytic activity was observed with a turnover number of up to 1.5 × 10. Furthermore, the Pd NP-OAc catalysts could be recycled at least five times.
在此，报道了以Pd(OAc)₂（= Pd(OCOCH₃)₂）作为纳米粒子前体合成新型N,N-二甲基甲酰胺（DMF）保护的钯纳米粒子（Pd NPs - OAc）。通过透射电子显微镜、傅里叶变换红外光谱、核磁共振和X射线光电子能谱对Pd NPs - OAc进行了全面表征，以确定钯纳米粒子的尺寸分布和DMF的配位状态。使用PdCl₂作为纳米粒子前体，将Pd NPs - OAc与Pd NPs - Cl进行了比较。在Pd NPs - OAc存在下，铃木 - 宫浦交叉偶联反应高效进行，观察到高达1.5×10³的周转数，具有高催化活性。此外，Pd NP - OAc催化剂至少可以循环使用五次。
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