Abstract

An original synthesis of pure (tetraphenylchlorinato)iron(III) chloride (1) is reported. Insertion of iron is achieved using 1.2 equivalents of cadmium acetate in DMF at 110°C, followed by a transmetallation reaction (in situ) using 8 equivalents of iron(II) chloride tetrahydrate in acetone at 60°C. The 1H NMR shifts at 25°C of the pyrrole protons varied from 60 to 100ppm. The absence of the signal at 80ppm related to undesired (tetraphenylporphirinato)iron(III) chloride is a purity criterion and shows the importance of the method used.Reaction of (tetraphenylchlorinato)iron(III) chloride (1) with four equivalents of tert-butyl isocyanide, 2,6-xylyl isocyanide and dimethylphenylphosphine in the presence of zinc amalgam in dichloromethane (DCM) afforded pure FeII(TPC)(t-BuNC)2 (2), FeII(TPC)(2,6-xylylNC)2 (3) and FeII(TPC)[P(Me)2Ph]2 (4) respectively.

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