Bis(eta-cyclopentadienyl) iron → N,N,N',N'-Tetramethylethylenediamine

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Reaction Steps

During a first step, ferrocene dilithium complexed with tetramethylethylenediamine (TMEDA) was prepared: In a glove box under argon, there is added 37 ml of freshly distilled TMEDA (247 mmoles) and 40 ml of anhydrous hexane in a 1 1 flask. There is then added drop wise 154 ml of a 1.6 M solution of butyllithium in hexane (247 mmoles, commercially available from Aldrich). After 10 min, there is added drop wise 18.6 g of ferrocene (100 mmoles) in solution in 500 ml of anhydrous hexane while keeping a strong stirring of the solution. After one night, orange crystals appeared in the solution, which were recovered by filtering the solution on a fritted glass of porosity No 4. After drying under vacuum, there is obtained 28.4 g of 1,1′-dilithio-ferrocene&Circlesolid;2 TMEDA (66% yield) which was preserved under argon.

Provenance & Evidence