The vic-dioximes are compounds with various industrial uses and scientific applications. Many coordination compounds have been synthesized based on vic-dioximes. This study presents the synthesis and full characterization of two vic-dioximes based on dichloroglyoxime, p-aminobenzoic acid, and p-aminotoluene. Their structures were proved by IR, ¹H, ¹³C and ¹⁵N 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 nonpathogenic gram-positive and gram-negative bacteria (Bacillus subtilis and Pseudomonas fluorescens), phytopathogenic (Xanthomonas campestris, Erwinia amylovora, E. carotovora) and the fungi (Candida utilis and Saccharomyces cerevisiae) at MIC – 70–150 μg/mL.