An efficient RuII‐catalyzed C−H bond redox‐neutral annulation of N‐nitrosoanilines with alkynes by employing water as the solvent has been developed. This transformation provides an easy and robust protocol for the synthesis of indoles with a broad range of functional group tolerance and excellent regioselectivity.

An efficient Rh(III)-catalyzed CÀ H activation and annulation cascade of primary benzylamines with readily accessible α-Cl ketones was developed. This transformation provides an easy and robust approach to diverse isoquinolines under air with broad functional group tolerance.

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An efficient Rh(III)‐catalyzed free NH2‐assisted C−H activation/cyclization of primary benzylamines with iodinium ylides was first developed. This transformation provides an easy approach to various dihydrophenanthridin‐1‐ones with broad functional group tolerance by using air as a green oxidant. Importantly, some reaction products exhibited some degree of growth inhibition of cancer cells.