We have synthesized 5-substituted-3-(3-substituted-4, 5-dihydroisoxazol-5-yl)-1, 2, 4-oxadiazole 4(a-f) and studied antimicrobial activities. The 5-substituted-1, 2, 4-oxadiazole were obtained by treating benzaldehyde oxime 1(a-c) with acrylonitrile in presence of oxidizing agent chloramine-T (CAT) to give isoxazoline 2(a-c), the isoxazoline 2(a-c) is react with NH2OH HCl in presence of Na2CO3 to give the corresponding isoxazoline-amidoxime 3(a-c). Finally, the amidoxime 3(a-c) coupled with aromatic acid in presence of coupling agent EDC. HCl to give isoxazoline-1, 2, 4-oxadiazole 4(a-f). The newly synthesized 1, 2, 4-oxadiazole 4(a-f) have been characterized by elemental analysis and spectral studies.