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Synthesis and characterization of cyclopentadienyl/alkoxo titanium dichlorides: structural analysis of monocyclopentadienyl titanium dichlorides with ligands derived from menthol and borneol

2004; Elsevier BV; Volume: 689; Issue: 22 Linguagem: Inglês

10.1016/j.jorganchem.2004.08.002

1872-8561

Yolanda Pérez, Sonia Morante‐Zarcero, Isabel del Hierro, Isabel Sierra, I. López-Solera, Magda Monari, Mariano Fajardo, Antonío Otero,

Carbon dioxide utilization in catalysis

A variety of monocyclopentadienyl alkoxo titanium dichloride and bisalkoxo titanium dichloride complexes have been prepared and characterized by spectroscopic techniques. The titanium derivatives containing both cyclopentadienyl and various alkoxo ligands [Ti(η5-C5H5)(OR)Cl2] (1–5) have been synthesized from the reaction of [Ti(η5-C5H5)Cl3] with 1 equivalent of the corresponding alcohol in THF in the presence of triethylamine (ROH = Adamantanol, 1R,2S,5R-(−)-menthol, 1S-endo-(−)-borneol, cis-1,3-(−)-benzylideneglycerol, 1,2:3,4-di-O-isopropylidene-α-d-galactopyranose). The bisalkoxo titanium dichloride derivatives [TiCl2(OR)2] (6–10) have been prepared by a redistribution reaction between Ti(OR)4 and TiCl4 compounds 6–8 (OR = Adamantanoxy, (1R,2S,5R)-(−)menthoxy, (1S-endo)-(−)-borneoxy) and by reaction of [Ti(OR)2(OPri)2]2 with CH3COCl compounds 9 and 10 (OR = 1,2:3,4-di-O-isopropylidene-α-d-galactopyranoxy, and 1,2:5,6-di-O-isopropylidene-α-d-glucofuranoxy). The molecular structures of 2 and 3 have been determined by single crystal X-ray diffraction studies.