REACTIONS OF (CYCLOPENTADIENYL)RHENIUM HALIDE-COMPLEXES (ETA-5-C5H5)RE(NO)(PPH3)(X) WITH NORMAL-BULI/TMEDA - GENERATION AND METHYLATION OF LITHIOCYCLOPENTADIENYL AND DILITHIOCYCLOPENTADIENYL LIGANDS
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Reactions of halide complexes (5C5H5)Re(NO)(PPh3)(X) [1, X = Cl (a), Br (b), I (c)] with nBuLi/TMEDA (1.1 equiv., THF, 78C) give lithiocyclopentadienyl complexes (5C5H4Li)Re(NO)(PPh3)(X) (2), as assayed by NMR and subsequent methylation to (5C5H4CH3)Re(NO)(PPh3)(X) (3). Reaction of 2a With further nBuLi/TMEDA affords (0C) dilithiocyclopentadienyl complex (51,3C5H3Li2)Re(NO)(PPh3)(Cl)(4), as assayed by NMR and methylation to [51,3C5H3(CH3)2]Re(NO)(PPh3)(Cl) (5). No significant migration of the halide ligand to the lithiocyclopentadienyl ligand is observed. New compounds 3ac and 5 are characterized by NMR (1H, 13C, 31P), IR, mass spectrometry, and microanalysis. Copyright 1988 WILEYVCH Verlag GmbH & Co. KGaA, Weinheim