Method B is the route of choice when aiming for a diaryliodonium salt with two electron-deficient and/or ortho-/meta-substituted aryl groups. One of the major challenges is to achieve complete oxidation of a low-reactive, electron-deficient iodoarene 1 in the presence of the weak Lewis acid BF3•OEt2. The original protocol has a pre-oxidation time of 15-60 minutes prior to the addition of the boronic acid to avoid decomposition of the organoboron reagent. However, iodoarenes 1 with strong (σp >0.60) or multiple EWG-substituents will not be efficiently oxidized within this time and we observed improved results when extending the pre-oxidation time to 90 min and the coupling time with the boronic acid 4 from 15 min to overnight (Scheme 4a). In this fashion, iodonium tetrafluoroborates 3o-3q could be isolated in moderate yields. It is nevertheless important to note that pre-oxidation times extended beyond 90 min will lead to decomposition and reduced yields