570401-36-4Relevant academic research and scientific papers
Synthesis and characterization of η5-tetramethylcyclopentadienyl- hydrido- and -chloro-silyl-η1-amido zirconium complexes
Vázquez, Ana Belén,Royo, Pascual
, p. 172 - 178 (2007/10/03)
The silylated tetramethylcyclopentadienes C5Me4 (SiMeCl2)(SiMe3) (1) and C5 Me4H(SiMeHCl) (3) were isolated by reaction of their corresponding trimethylsilyltetramethylcyclopentadienyl and tetramethylcyclopentadienyl lithium salts with SiMeCl3 and SiMeHCl2, respectively. Reaction of a toluene suspension of ZrCl4 with one equivalent of 1 afforded the monocyclopentadienyl zirconium complex [Zr(η5- C5Me4SiMeCl2)Cl3] (2). Reaction of 3 with NH2tBu gave C5Me4H[SiMeH(NHtBu)] (4) which was further metallated to give Li2[C5 Me4SiMeH(NtBu)] (5), used to prepare the silyl-η1-amido zirconium derivative [Zr(η5-C5Me4 SiMeH-η1-NtBu)Cl2] (6) by reaction with ZrCl4(THF)2. Chlorination of 6 with BCl3 afforded [Zr(η5-C5 Me4SiMeCl-η1-NtBu)Cl2] (12). Alkylation and amidation of 6 and 12 provided the corresponding disubstituted [Zr(η5-C5Me4 SiMeH-η1-NtBu)R2] (R=Me 7, CH2Ph 8, NMe2 (9) and [Zr(η5-C5Me4 SiMeCl-η1-NtBu)Me2] (13) and monosubstituted [Zr(η5-C5Me4 SiMeH-η1-NtBu)ClR] (R=C6F5 10, N(SiMe3)2 (11) and [Zr(η5-C5Me4 SiMeCl-η1-NtBu)Cl{N(SiMe3) 2}] (14). All of the new compounds reported were characterized by elemental analyses and NMR spectroscopy.
