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The introduction of microwave irradiation in organic synthesis has revolutionized traditional synthetic chemistry by enhancing efficiency, reducing reaction times, lowering costs, improving selectivity, increasing safety, and promoting sustainability. Consequently, microwave technology has become indispensable in diverse fields, including the synthesis of peptides, biologically active heterocycles, industrially valuable organic compounds, polymers, and materials science. The use of microwave heating has significantly advanced the synthesis of biologically relevant organic sulfides/thioethers and disulfides compared to conventional synthetic routes. These methods offer shorter reaction times, excellent yields, simple work-up procedures, and the use of green solvents or solvent-free and metal-free reaction conditions, making them more attractive from a green chemistry perspective. Moreover, microwave heating simplifies the solid-phase synthesis of disulfide-rich peptides, making it more viable, selective, and cost-effective. Notably, substantial progress has been made over the past two decades in synthesizing small molecules of both symmetrical and unsymmetrical organic sulfides and disulfides, including disulfide-containing therapeutic peptides, under microwave irradiation. This review provides an overview of recent advancements in the microwave-assisted synthesis of a wide variety of bioactive diaryl and aryl–alkyl sulfides and disulfides, including a disulfide-bridged cycloheptapeptide, along with critical discussions where necessary.
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