A series of 3, 5-bis (indolyl)-1, 2, 4-thiadiazoles were synthesized and evaluated for their cytotoxicity against selected human cancer cell lines. The reaction of indole-3- thiocarboxamide 3 with iodobenzene diacetate underwent oxidative dimerization to give 3, 5- bis (indolyl)-1, 2, 4-thiadiazoles 4a–n. Among the synthesized bis (indoly)-1, 2, 4- thiadiazoles, the compound 4h with 4-chlorobenzyl and methoxy substituents showed the ...