An Undergraduate Experiment Using Microwave-Assisted Synthesis of First Raw Metalloporphyrins: Characterizations and Spectroscopic Study

Abstract

There is a notable absence in the practical inorganic curricula for experiments in which students can synthesize and characterize series of inorganic complexes. This is possibility attributed to the long required time which is not normally available in regular lab sessions. To address this absence, this paper describes a two-part experiment for chemistry major students in which they prepare series of metalloporphyrins using microwaveassisted technique. In addition to its attractive simplicity, microwave-assisted preparation substantially reduces the needed reaction time to suit the lab session duration. The first lab session is dedicated to the characterization of the 5,10,15,20-tetraphenylporphyrin (TPP) as well as the synthesis of the corresponding Fe(II), Co(II), Ni(II), Cu(II) and Zn(II) complexes. The second session involves the spectroscopic characterization (UV-vis, 1H-NMR, and IR) of the prepared metalloprophyrins. The students relate the experimental results with the provided theoretical data based on quantum chemical calculations.