Abstract

The tricarbonyl(cyclobutabenzene)chromium(O) complexes 12 – 20, have been prepared from the free ligand and triammintricarbonylchromium(O) or hexacarbonylchromium(O). The complexes have been characterized by spectroscopic methods (IR, 1H NMR, 13C NMR) and mass spectrometry, and 1H‐NMR signal assignments have been verified by an NOE experiment. Diastereomeric ratios have been determined by 1H NMR and the diastereomers of the 1‐methyl derivative 16 separated by HPLC. A crystal‐structure analysis is presented for exo;‐16. A photochemical ligand exchange takes place in 70% yield for the 1‐trimethylsilyl derivative 19. Metalation with n‐butyl‐lithium/tmeda at –78°C has been observed only for the aromatic and not for the benzylic protons.

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