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A novel series of 5‐substituted/unsubstituted [1,2,4]triazolo[3,4‐b][1,3,4] thiadiazine compounds has been achieved successfully through chemoselective reduction of the C = N bond, based on our prior work. Initial biological evaluation illustrated that the most active derivative 7j exhibited significant cell growth inhibitory activity toward MCF‐7, A549, HCT116, and A2780 with the IC50 values of 0...