4.6 Article

Mechanochemical synthesis of half-sandwich iridium/rhodium complexes with 8-hydroxyquinoline derivatives ligands

Journal

APPLIED ORGANOMETALLIC CHEMISTRY
Volume 36, Issue 4, Pages -

Publisher

WILEY
DOI: 10.1002/aoc.6588

Keywords

catalyst; half-sandwich metal complex; mechanochemistry; structure

Funding

  1. Natural Science Foundation of Anhui Province [2008085QB60]
  2. National Natural Science Foundation of China [21102004]

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Mechanochemistry provides a rapid and efficient method for the synthesis of half-sandwich iridium and rhodium complexes, and post-synthetic modification can be carried out to alter their structures. The half-sandwich rhodium complexes exhibit high catalytic activity towards the amide synthesis between aldehydes and hydroxylamine hydrochloride.
Mechanochemistry provides a rapid, efficient route to half-sandwich iridium and rhodium complexes from [MCp*(mu-Cl)Cl](2) (M = Ir, Rh) and 8-hydroxyquinoline-2-carbaldehyde without the need for Schlenk manipulation, inert gas protection, or dry solvents. Furthermore, post-synthetic modification of the half-sandwich metal complexes has been carried out via a mechanochemical Wittig reaction between half-sandwich metal complex and phosphorus ylide. All complexes were fully characterized by H-1 and C-13 NMR spectra, infrared spectroscopy, mass spectrometry, and single-crystal X-ray diffraction method. The half-sandwich rhodium complexes exhibited high catalytic activity towards the amide synthesis between aldehyde and hydroxylamine hydrochloride (NH2OH center dot HCl) with a broad functional group tolerance.

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