The synthesis of a series of polymethylene chain‐bridged aminochloropyrimidines as potential DNA intercalators is described. N,N'‐Bis(2‐amino‐6‐chloro‐4‐pyrimidyl)‐1,3‐diaminopropane ( 3 ), N,N'‐bis(2‐amino‐6‐chloro‐4‐pyrimidyl)‐1,4‐diaminobutane ( 4 ), N,N'‐bis(2‐amino‐6‐chloro‐4‐pyrimidyl)‐1,6‐diaminohexane ( 5 ), N,N'‐bis(2‐amino‐6‐chloro‐4‐pyrimidyl)‐1,8‐diaminooctane ( 6 ), N,N'‐bis(2‐amino‐6‐chloro‐4‐pyrimidyl)‐1,10‐diaminodecane ( 7 ), and N,N'‐bis(2‐amino‐6‐chloro‐4‐pyrimidyl)‐1,12‐diaminododecane ( 8 ) were synthesized from 2‐amino‐4,6‐dichloropyrimidine ( 1 ) and 1,3‐diaminopropane, 1,4‐diaminobutane, 1,6‐diaminohexane, 1,8‐diaminooctane, 1,10‐diaminodecane, and 1,12‐diaminododecane, respectively. The spectral data and other physical properties of the new compounds are discussed.