A Robust Synthesis of Fluorosurfactants with Tunable Functionalities via a Two‐Step Reaction

Abstract Fluorosurfactant‐stabilized microdroplets hold significant promise for a wide range of applications, owing to their biological and chemical inertness. However, conventional synthetic routes for fluorosurfactants typically require multiple reaction steps and stringent conditions, such as high temperatures and anaerobic environments. This complexity poses a significant limitation to the development of fluorosurfactant synthesis and its subsequent applications in droplet‐based systems. In this work, a robust two‐step synthesis of fluorosurfactants with tunable functionalities is presented. Microdroplets stabilized by these fluorosurfactants exhibit enhanced stability and biocompatibility. Notably, these fluorosurfactants facilitate the formation of nanodroplets that efficiently transport and concentrate fluorophores with high selectivity. Furthermore, it is demonstrated that colloidal self‐assemblies with distinct structures can be engineered by modulating interactions between the fluorosurfactants and colloidal particles. The synthetic approach provides a strategy for the rapid production of functional fluorosurfactants under mild conditions, enabling droplet‐based microfluidic techniques with applications in biology and material science.