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Article Dans Une Revue Inorganica Chimica Acta Année : 2013

Synthesis of pure iron(II) mesotetraphenylchlorin complexes via a versatile general method of iron insertion into chlorins

Marwan Kobeissi
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Khalil Cherry
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Mahmoud K. Faraj
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Résumé

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 100 ppm. The absence of the signal at 80 ppm 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.

Dates et versions

hal-00871915 , version 1 (11-10-2013)

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Marwan Kobeissi, Khalil Cherry, Mahmoud K. Faraj, Gérard Simonneaux. Synthesis of pure iron(II) mesotetraphenylchlorin complexes via a versatile general method of iron insertion into chlorins. Inorganica Chimica Acta, 2013, 396, pp.30-34. ⟨10.1016/j.ica.2013.01.012⟩. ⟨hal-00871915⟩
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