Automated One‐Pot Library Synthesis with Aldehydes as Radical Precursors

Abstract The increased demand for the synthesis of Csp 3 enriched motifs and the urgency of discovering new drugs requires the development of more efficient technologies and synthetic tools to accelerate drug discovery processes. Herein, we report a fully automated strategy for the addition of Csp 3 enriched building blocks onto olefins via Giese addition to forge Csp 3 −Csp 3 bonds. The developed fully automated protocol allowed the in‐situ conversion of aldehydes (non‐redox‐active species) to electroactive imidazolidines and their use as precursors of C‐centered radicals under photoredox catalyzed conditions for the synthesis of building blocks and bioactive compound libraries by synthesizing sp 3 ‐enriched compounds.