The vic-dioximes are compounds with various industrial uses and scientific applications. Many coordination compounds have been synthesized based on vicdioximes. This study presents the synthesis and full characterization of two vicdioximes based on dichloroglyoxime, p-aminobenzoic acid and p-aminotoluene. Their structures were proved by IR, 1 H, 13 C and 15 N NMR spectral analysis and single crystal X-ray diffraction. One of the reported vic-dioximes, bis(di-p-aminotoluene)glyoxime mono-p-aminotoluene trihydrate showed good to moderate antimicrobial activity against both non-pathogenic Gram-positive and Gram-negative bacteria (Bacillus subtilis and Pseudomonas fluorescens), phytopathogenic (Xanthomonas campestris, 2 Erwinia amylovora, E. carotovora) and the fungi (Candida utilis and Saccharomyces cerevisiae) at MIC -70-150 μg/mL.