Abstract

GIRALDO LONDONO, Cristian Camilo et al. Palladium nanoparticles supported in laminar hydroxide salts: potential use in Sonogashira reactions. Rev.Colomb.Quim. [online]. 2017, vol.46, n.2, pp.51-65. ISSN 0120-2804.  https://doi.org/10.15446/rev.colomb.quim.v46n2.63028.

This article reports the synthesis of palladium nanoparticles supported on zinc acetate hydroxysalts and modified with a surfactant (LHS-Zn-Ac/Pd0 and LHS-Zn-Suf/Pd0 respectively), by insertion of [PdCl4]2- and its subsequent reduction with ethanol at reflux. With the surfactant insertion, the interlaminar distance of the starting hydroxysalt (LHS-Zn-Ac) increased from 13.8 Å to 29.8 Å, while the final materials containing palladium metal registered interlaminar distances of 22.4 Å and 29.4 Å for LHS-Zn-Ac/Pd0 and LHS-Zn-Suf/Pd0 respectively. Zinc acetate hydroxysalt and surfactant with incorporated palladium metal nanoparticles were tested as potential catalysts in the Sonogashira reaction starting from phenylacetylene and aryl iodides, particularly iodobenzene or 2-iodophenol, giving diphenylacetylene (32% yield of isolated and purified product) or 2-phenylbenzofuran (18%). All inorganic materials were characterized by the following techniques: X-ray diffraction (XRD), scanning electron microscopy (SEM and SEM-EDS), transmission electron microscopy (TEM) and Fourier transformed infrared spectroscopy (FT-IR). The organic compounds were characterized by nuclear magnetic resonance (1H-NTMR and 13C-NMR) and gas chromatography coupled to mass spectrometry (GC-MS).

Keywords : Hydroxide salts; sodium lauryl sulfate; palladium nanoparticles; Sonogashira C-C coupling reactions; diphenylacetylene; 2-phenylbenzofuran.

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