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Abstract : A new series of acylselenourea, i.e., 4-Nitro-N-((4-(N-(pyrimidin-2-yl) sulfamoyl) phenyl) carbamoselenoyl) Benz amide(1), 4-Methyl-N-((4-(N-(pyrimidin-2-yl) sulfamoyl) phenyl) carbamoselenoyl) Benz amide(2), 4-Nitro-N-((4-nitrophenyl) carbamo selenoyl) Benz amide(4), N-(2,6-dioxo-1,2,3,6-tetrahydropyrimidine-1-carbonoselenoyl)-4-nitrobenzamide(5), these compounds were prepared from reaction of KSeCN with 4-Nitrobenzoyl chloride in dry THF followed by adding appropriate anime compound in situ, i.e. sulfadiazine, 4-Nitroaniline and Uracil. One acylthiourea derivative, i.e., 4-Methyl-N-((4-(N-(pyrimidin-2-yl) sulfamoyl phenyl) carbamothioyl) Benz amide(3)was prepared from reaction of 4-Methylbenzoyl chloride with KSCN in dry THF followed by addition of sulfadiazine in situ. All prepared compounds were characterized by FT-IR, CHNS, 1H-NMR and 13C-NMR spectroscopic data which confirm the proposed structures for the prepared compounds.