Several per-O-acetyl and per-O-benzoyl glycosylbis-thiocarbamides were synthesized by the interaction of glycosylisothiocyanates and o-phenylenediamine. The identities of these newly synthesized compounds were established on the basis of usual chemical transformations, IR, 1H NMR, 13C NMR and Mass spectral studies. All the synthesized compounds have been evaluated for their antibacterial and antifungal activity against different bacteria and fungi by agar diffusion method.