Abstract The carbon─sulfur (C─S) bond is an essential structural unit in various therapeutic agents, including antibiotics and anticancer drugs. C─S coupling reactions involving organothiols and aryl electrophiles have emerged as a powerful strategy. Recently, C─S coupling using heterogeneous catalysts like metals, metal oxides, and single‐atom sites on polymers, 2D materials, and nanoporous metal‐organic frameworks (MOFs) has shown promise due to synergistic properties enhancing nanoscale dispersion, stability, activity, recyclability, and control over key textural parameters. This review highlights the design, synthesis, and catalytic behavior of nanomaterials and their supports for C─S coupling reactions. Particular attention is given to a critical evaluation of the emergence of advanced materials, including a comprehensive discussion of the underlying reaction mechanisms and an in‐depth analysis of advanced materials to enhance catalytic activity, selectivity, and stability. Furthermore, mechanistic insights derived from density functional theory calculations are discussed to support the rational design and development of efficient and selective catalysts. Finally, recent advancements, emerging trends are summarized, and strategic insights for the design of next‐generation catalysts with enhanced efficiency in C─S bond‐forming transformations are offered.
Lo et al. (Sun,) studied this question.
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