Site‐Selective Phosphonation of Arenes via Hypervalent Iodine‐Mediated C─H Functionalization

A white light‐promoted, metal‐free strategy based on hypervalent iodine‐mediated C─H functionalization was developed for the synthesis of aryl phosphonates. This method facilitates the straightforward conversion of an array of arenes into their respective diaryliodonium salts, which are subsequently subjected to a metal‐free phosphonation process to yield structurally diverse aryl phosphonates. Furthermore, the practical synthetic value of this approach was demonstrated through its application in the late‐stage structural diversification of complex molecules.