Some new substituted acetophenone 4-(2,3,4,6-tetra-O-acetyl-beta-D-galactopyranosyl)thiosemicarbazones 4 were synthesized by reaction of 4-(2,3,4,6-tetra-O-acetyl-beta-D-galactopyranosyl) thiosemicarbazide 2 and substituted acetophenone 3. The reaction was performed using microwave-assisted method. The structure of obtained products was confirmed by spectroscopic methods (such as IR, 1H and 13CNMR, MS).