A series of diolate-substituted diboron compounds were investigated as reagents for iridium-catalyzed C–H borylations of arenes. These studies showed that commercially available bis(hexylene glycolato)diboron reacts with arenes in the presence of the catalyst generated from [Ir(COD)OMe]<sub>2</sub> and di-<i>tert</i>-butylbipyridine. This reagent is prepared from a less expensive diol than the more commonly used bis(pinacolato)diboron reagent.
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