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The reaction of bis(trimethylsilyl) sulfide with different substituted thiiranes under tetrabutylammonium fluoride (TBAF) catalysis leads to the synthesis of 3,7‐disubstituted‐1,2,5‐trithiepanes, through regioselective reaction of a thiosilane intermediate with another molecule of episulfide, followed by intramolecular oxidation of two sulfur units. When using bis(trimethylsilyl)selenide, the reaction...