An advanced level undergraduate lab is described in which a hypervalent iodine(III) compound, (dichloroiodo)benzene, is synthesized and the kinetics and thermodynamics of ligand-exchange with (diacetoxyiodo)benzene is studied by <sup>1</sup>H NMR spectroscopy. The lab has three components. The first involves a kinetic study of the chlorination of a monovalent iodine compound, iodobenzene, with sulfuryl chloride, and extraction of the pseudo-first order rate constant. The compound is then synthesized on a larger scale, isolated, and characterized spectroscopically. The last component is a kinetic study of the formation of a mixed-ligand hypervalent iodine compound, PhI(Cl)OOCCH3, from the (dichloroiodo)benzene synthesized in the second part and the commercially available (diacetoxyiodo)benzene. The collected data are used to calculate both rate and equilibrium constants of the ligand exchange. In this lab, students learn about the concept of hypervalent bonding, how to properly conduct kinetic studies and process kinetic data, as well as experimental methods for determining rate and equilibrium constants.

Advanced undergraduate lab: Kinetics and thermodynamics of formation of hypervalent iodine compounds

2019 Fall National Meeting

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