There remain several key challenges to existing therapeutic systems for cancer therapy, such as quantitatively determining the true, tissue-specific drug release profile in vivo, as well as reducing side-effects for an increased standard of care.

The development of practical routes that enable the synthesis of unimolecular non‐natural macromolecules on multi‐gram scales remains a key challenge in polymer chemistry. Herein, we present a continuous flow setup employing the light‐induced chemistry based on photocaged dienes as a controlled ligation system to establish a new platform for scalable monodisperse macromolecular synthesis. 800 mg of sequence‐defined linear chains with 8 repeating units were obtained in a sequential protecting group based 2‐step process. The current study demonstrates that photoflow synthesis is a viable approach to generate large quantities of monodisperse oligomers.

Scheme 1. Overview of the two-colour photoflow setup. Consecutive irradiation of the compounds with UV-A light (l 1 = 350 nm) and violetblue light (l 2 = 410 nm), respectively, selectively folds the polymeric chains into macrocycles.

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