Abstract Dimercaptans and diamines react with 3-bromo-N-tritylpropanamine to give the corresponding N, N′-ditrityldithia and N, N′-ditritylpolyaza compounds in yields of 50– 80%. The trityl protecting groups are readily removed in acid. These reactions make possible the synthesis of a number of new α-ω-diamino compounds needed for the synthesis of new dithiadiaza, di-and polyaza macrocyclic ligands.