In the synthesis of diaryliodonium triflates (Route A with TfOH), the general addition order of the reagents should be addressed. In the original protocol, iodoarene 1 and arene 2 are added together with m-CPBA in CH2Cl2 followed by the acid. To avoid undesired oxidation of 2 with electrondonating groups (EDG), the reaction can be performed as a sequential one-pot reaction with initial oxidation of 1 to iodine(III)intermediate 5 followed by addition of 2 (Scheme 2). If the iodoarene 1 bears strong electron withdrawing groups (EWG), the oxidation of the iodine will be slow and pre-oxidation of 1 for 10-60 minutes prior to the addition of 2 greatly enhances the yield. This modification has proven beneficial in reactions of iodoarenes 1 bearing ortho-F and meta-EWG substituents with moderately electron rich arenes 2 to yield products 3a-f (Scheme 2a). With stronger electron donating properties of arene 2, only pre-oxidation of 1 is not sufficient to overcome this issue. In a previous method, we reported that N-heterocyclic anisyl salts could be synthesized through the addition of water to quench the excess triflic acid prior to the addition of arene 2. In this update, we emphasize the applicability of this additive in the synthesis of a broader scope of unsymmetric diaryliodonium salts with electron-rich dummy groups like anisyl and thiophenyl. Even using highly electron-deficient substrates 1, undesired oxidization of 2 can be avoided by water addition, resulting in the synthesis of iodonium salts 3g, h in good yields (Scheme 2b).