Functionalization of Complexed N2O in Bis(pentamethylcyclopentadienyl) Systems of Zirconium and Titanium.
作者： Daniel J. Mindiola , Lori A. Watson , Karsten Meyer , Gregory L. Hillhouse
DOI: 10.1021/OM5002556
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摘要: Methyl triflate reacts with the metastable azoxymetallacyclopentene complex Cp*2Zr(N(O)NCPhCPh), generated in situ from nitrous oxide insertion into Zr–C bond of Cp*2Zr(η2-PhCCPh) at −78 °C, to afford salt [Cp*2Zr(N(O)N(Me)CPhCPh)][O3SCF3] (1) 48% isolated yield. A single-crystal X-ray structure 1 features a planar azoxymetallacycle methyl alkylation taking place only β-nitrogen position former Zr(N(O)NCPhCPh) scaffold. In addition 1, methoxy-triflato Cp*2Zr(OMe)(O3SCF3) (2) was also reaction mixture 26% yield and fully characterized, including its independent synthesis Cp*2Zr═O(NC5H5) MeO3SCF3. Complex 2 could be observed, spectroscopically, thermolysis (80 days). contrast Cp*2Zr(N(O)NPhCCPh), more stable titanium N2O-inserted analogue, Cp*2Ti(N(O)NCPhCPh), MeO3SCF3 1:1 regioisomeric salts, [Cp*2Ti(N(O)N(Me)CPhCPh)][O3SCF3] (3) [Cp*2Ti(...
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