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Synthesis of Ruthenocene, [l.l]Ferroceno-Ruthenocenophane and [l.l]Ruthenocenophane Using Di-Ruthenium(II)-Tetracarboxylates

1993; Taylor & Francis; Volume: 23; Issue: 4 Linguagem: Inglês

10.1080/15533179308016660

1532-2440

Ulrich T. Mueller‐Westerhoff, Gerhard F. Swiegers,

Metal complexes synthesis and properties

Abstract A new synthetic route to ruthenocene, [1.1]ferroceno-ruthenocenophane, and [1.1]ruthenocenophane involves the use of ruthenium(II) carboxylates, (Ru2OCR)4,R = C3H7 and C7H15), the metal source and does not, as most alternate sytheses do, require an excess of the ligand. The long chain chloro-Ru(II,III) carboxylates were obtained from chloro-ruthenium(II,III) tetraacetate by reaction with the respective carboxylic acids and were subsequently reduced to the Ru(II,II) species. Ruthenocene was produced in >90% yield by reacting either of these carboxylates with stoichiometric amounts of sodium cyclopentadienide. The synthesis of the metallocenophanes involved addition of the Ru(II) carboxylate to the dianions of 1,1′-bis(cyclopenta-dienylmethyl) ferrocene or 1,l′-bis(cyclopentadienyl-methyl)ruthenocene and produced 11–12% yields of the two cyclic systems. Considerable amounts of the dimers (Cp-CH2-Cp)4M4 were formed in these reactions.