Suzuki Coupling Reaction Catalyzed by Palladium Supported on Mesoporous Titanium Dioxide in Continuous Flow
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the Fundamental Research Funds for the Central Universities (5032101201702) ; Program of Leading Talents (2013)

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    Abstract:

    0.1 wt%~1.0 wt% heterogeneous Pd/m-TiO2 catalysts were prepared by Sol-Gel method using PdCl2 and n-butyl titanate as raw materials, PVP as metal protective agent, F127 as template agent. The structure was characterized by BET, XRD and TEM. The results showed that the catalysts had an ordered mesoporous structure with 8 nm~10 nm pore size distribution, 11.3 nm~13.3 nm palladium particle size and good dispersion. Then Pd/m-TiO2 catalyst was fixed by micro-packed reactor to catalyzed Suzuki coupling reaction in continuous flow. The optimal continuous flow process was determined: mixed solvent of DMF and water (V:V=1:1, 400 mL), base K3PO4(n碱:n溴苯=1.5:1) , 0.20 mL/min flow rate, 0.10 mol/L bromobenzene, 0.12 mol/L phenylboronic acid, 0.15 mol/L K3PO4, 0.7 wt% palladium loading and 80 ℃ reaction temperature. The yield of Suzuki coupling reaction was 99% in 6.8 min residence time. The catalyst still maintained good catalytic activity after repeated use.

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History
  • Received:March 03,2021
  • Revised:April 06,2021
  • Adopted:April 07,2021
  • Online: July 13,2021
  • Published: