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Diazo anhydrides (ArNNONNAr) have been known since 1896 but have rarely been used in synthesis. This communication describes the development of a photochemical catalyst‐free CH arylation methodology for the preparation of bi(hetero)aryls by the one‐pot reaction of anilines with tert‐butyl nitrite and (hetero)arenes under neutral conditions. The key step in this procedure is the in situ formation...
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