The construction of C(sp3)‐sulfonyl bonds through direct sulfonylation of C(sp3)−H bond presents a number of challenges, so an electrochemical oxidation‐induced direct sulfonylation of the xanthene C(sp3)−H bond was developed. Significant advantages of this method are high atom efficiency, functional group tolerance, transition metal‐ and oxidant‐free conditions. The in vitro cytotoxicity of all product is evaluated by MTT assay against human cancer cell lines. The results reveal that most of the compounds 3 da and 3 af have good inhibitory activity on tumor cell lines.
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