Sistemas catalíticos heterogêneos para reações de acoplamento Stille-Migita
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2019-08-27
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Universidade Federal de Goiás
Resumo
Carbon-carbon coupling reactions are of fundamental importance in the synthesis of organic
compounds. The Stille-Migita reaction is a cross-coupling reaction and occurs when an organotin compound and an organic halide hybridized to sp3 react under the presence of a metal-based catalyst, generally palladium. The reaction has the advantage of being compatible with virtually any functional group and for forming products with complex chains, such as pharmaceuticals and agrochemicals. However, Stille synthesis is usually performed by homogeneous catalysis, which enhances the need for costly purification processes necessary to remove metal debris from the reaction products. Thus, this work synthesized and verified the use of heterogeneous catalysts for Stille coupling reactions, using the
efficient and economical method of wet impregnation in its preparation by producing monometallic catalysts with different oxides as support. The catalysts were characterized before and after calcination by thermogravimetry and differential thermal analysis (TG / DTA), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), textural analysis by adsorption/desorption isotherms of N2 and X-ray fluorescence (XRF). The reaction parameters were optimized: time, temperature, type of solvent and catalyst composition. The materials La2O3/Pd and TiO2/Pd showed no catalytic activity, whereas the catalysts Nb2O5/Pd and SiO2/Pd showed good conversions, above 80%. The recycling tests showed
considerable loss of activity, which could be associated with filtration and leaching of the active phase between cycles. Nb2O5/Pd showed higher efficiency in the presence of non-toxic solvents (water/ethanol), unusual in Stille reactions. It is expected that this work will contribute to the development of heterogeneous catalysis, particularly in the coupling reactions, since economical methods of synthesis have produced catalytically active materials.
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GODOY, P. H. M. Sistemas catalíticos heterogêneos para reações de acoplamento Stille-Migita. 2019. 132 f. Dissertação (Mestrado em Engenharia Química) - Universidade Federal de Goiás, Goiânia, 2019.