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Herein, we have reported a straightforward methodology for the synthesis of dithioacetals through a metal‐free catalyzed reaction of aldehydes with thiols. In this regard, sulfamic acid proved to be a very efficient catalyst for the preparation of desired products under conventional heating as well as ultrasound irradiation. Generally, the desired products were obtained with reasonable yields through a thioacetalization process, under mild reaction conditions. Noteworthy, sulfamic acid could be recovered from the reaction by simple filtration and it was reused in further reactions and it showed good catalytic activity until the third cycle. In addition, a series of control experiments have also been performed and a plausible reaction mechanism has been illustrated.

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This manuscript portrays the CuI-catalyzed Csp-chalcogen bond formation through cross-coupling reactions of propynyl esters and diorganyl dichalcogenides by using DMSO as solvent, at room temperature, under base-free and open-to-air atmosphere. Generally, the reactions have proceeded very smoothly, being tolerant to range of substituents present in both substrates, affording the novel 3-(organochalcogenyl)prop-2-yn-1-yl esters in moderate to good yields. Noteworthy, the 3-(butylselanyl)prop-2-yn-1-yl benzoate proved to be useful as synthetic precursor in palladium-catalyzed Suzuki and Sonogashira type cross-coupling reactions by replacing the carbon-chalcogen bond by new carbon-carbon bonds. Moreover, the 3-(phenylselanyl)prop-2-yn-1-yl benzoate has shown promising in vitro activity against glioblastoma cancer cells.

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