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A series of new bis sulfonamide/carbamate derivatives of bis‐(4‐aminophenyl)methane 3(a–d)/5(a–f) were synthesized from bis‐(4‐aminophenyl)methane (1) using various pharmacologically active sulfonyl chlorides 2(a–d) and carbonochloridates 4(a–f) in high yields. The structures of all the newly synthesized compounds were characterized by the Infrared spectroscopy, NMR (1H and 13C), mass, and elemental analyses. Further, all the synthesized compounds were tested for the antioxidant activity by using 2, 2‐diphenyl‐1‐picrylhydrazyl, NO, and H2O2 scavenging methods and antimicrobial activity. Most of the compounds exhibited good antioxidant and antimicrobial activities. [ABSTRACT FROM AUTHOR]