High yield synthesis of oxo-tungsten(V) porphyrin: Structural characterization of the hydrolyzed products

Thermal reaction of [W(NO)2(py)2(Cl)2] and TTPH2 in 1:1 stoichiometric ratio in the solid matrix of 4-chlorobenzoic acid resulted the formation of complex [WVO(TTP)((4-ClBZ)] (1) (where 4-ClBz = 4-chlorobenzoate ion and TTP = dianion of 5,10,15,20-meso-tetratolyporphyrin) in almost quantitative yield. The synthesized complex is characterized by different spectroscopic techniques like UV–Vis, FT-IR, ESR, ESI mass and by electrochemical studies. 1 on chromatographic purification stage using alumina column is hydrolyzed in the presence of traces of moisture present in the DCM/ethyl acetate and DCM/methanol used as the eluting solvent mixture leading to the formation of trans oxo-hydroxo and oxo-methoxo complexes respectively. The hydrolyzed complexes show varied electrochemical behavior compared to 1.