Synthesis and Structural Verification of an ArI(OTf)2

PhI(OTf)2 and related ArI(OTf)2 species have been incorrectly invoked as intermediates in oxidation reactions for many years. We recently established that such compounds did not yet exist but remain an attractive target. Here we describe the synthesis, isolation and structural characterization of NO2-PhI(OTf)2 which is resistant to decomposition, and also more reactive than PhI(OTf)(OAc), the species previously misidentified as PhI(OTf)2.