For the purpose of studying the relation between molecular structure and tuber-culostatic activity in the acylthiosemicarbazide group,some new derivatives of thiosemi-carbazide have been synthesized.When aroylisothiocyanate reacted with arylhydrazines or isonicotinoyl hydrazide in dioxane or acetonitrile,the corresponding 1-aryl-4-aroyl-thiosemicarbazides(Ⅰ) and 1-isonicotinoyl-4-amyl-thiosemicarbazides(Ⅱ) were formed respectively in yields of 50-90%(see Tables 1 and 2 in the Chinese text).