New αω-bis-(2-hetaryl-4-oxothiazolidin-3-yl)alkanes were prepared via a common two step procedure using N,N-bis-hetarylidenamines condensation with α-mercaptoacetic acid. The used bis-aldimines were obtained from reaction between ethylenediamine or putrescine and benzaldehyde or the isomeric pyridinecarboxyaldehydes. The bis-(2-phenyl-4-oxothiazolidin-3-yl)alkanes were prepared by one-pot three component reaction of diamine, aldehyde and α-mercaptoacetic acid under very mild conditions.