Abstract 4, 7-Decadienal, 4, 7-tridecadienal, 5, 8-tetradecadienal and 6, 9-dodecadienal (all- cis) have been synthesized by coupling 1-bromo-2-pentyne and 1-bromo-2-octyne with the diethyl acetals of 4-pentynal, 5-hexynal and 6-heptynal, followed by partial hydrogenation and hydrolysis. The formation of 1, 1, 4-triethoxy-2, 5-hexadiyne from 1, 1-diethoxy-2- propyne is also described.