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Synthesis and spectroscopic characterization of titanium pyridylanilido complexes as catalysts for the polymerization of 1,3-butadiene and isoprene

Inorganica Chimica Acta, ISSN: 0020-1693, Vol: 487, Page: 331-338
2019
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A series of titanium(IV) complexes of general formula TiCl 3 [ N,N -(pyridin-2-ylalkyl)anilido, TiCl 3 L, 8 – 13, were prepared by reactions of TiCl 4 with substituted (pyridin-2-ylalkyl)anilines, L H, and characterized by analytical and spectroscopic methods. Compound 10 was obtained by using TiI 4 as titanium precursor. In the case of L H  = 2,6-diisopropyl(pyridin-2-ylmethyl)aniline, 1, and 2,6-diisopropyl(pyridin-2-ylethyl)aniline, 2, the intermediate formation of TiCl 4 L H, 6 – 7, was detected, undergoing HCl elimination on heating to finally give 8 and 9. The products are not stable in coordinating solvents (thf, CH 3 CN). Ligand dissociation was observed from TiCl 3 ( N,N -2,6-diisopropyl(pyridin-2-ylmethyl)anilido, 8, resulting in the formation of Ti 2 OCl 6 (CH 3 CN) 4 and 2-(2,6-diisopropyl-phenylaminomethyl)pyridinium hexachlorotitanate. By reaction of TiCl 3 (thf) 3 or TiI 3 with 1 and 2 at ca 100 °C, the air sensitive derivatives TiCl 2 L, 14, and TiI 2 L, 15, were afforded. All titanium complexes were evaluated as catalysts for the polymerization of 1,3-butadiene and isoprene, in association with methylaluminoxane (MAO). The results indicate that the catalytic activity is strictly dependent on the nature of the ligands and the oxidation state of the metal, while the nature of the titanium complex has negligible influence on the selectivity.

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