Efficient and General One‐Pot Synthesis of Diaryliodonium Triflates: Optimization, Scope and Limitations

Abstract Symmetrical and unsymmetrical diaryliodonium triflates have been synthesized from both electron‐deficient and electron‐rich arenes and aryl iodides with m CPBA and triflic acid. A thorough investigation of the optimization, scope and limitations has resulted in an improved one‐pot protocol that is fast, high‐yielding, and operationally simple. The reaction has been extended to the direct synthesis of symmetrical iodonium salts from iodine and arenes, conveniently circumventing the need for aryl iodides.