202007-67-8Relevant academic research and scientific papers
Synthesis of pure iron(II) mesotetraphenylchlorin complexes via a versatile general method of iron insertion into chlorins
Kobeissi, Marwan,Cherry, Khalil,Faraj, Mahmoud K.,Simonneaux, Gérard
, p. 30 - 34 (2013)
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 Fe II(TPC)[P(Me)2Ph]2 (4) respectively.
