A scheme is developed for the high-yield synthesis of polyamine catecholamides from the secondary N-benzylamines N% enzylhomospermidine, N4-benzylspermidine, and NJ-bis (3- aminopropy1) benzylamine. These amines are first selectively acylated at the N-terminal positions with 2, 3-dimethoxybenzoyl chloride, and the benzyl groups are removed by hydrogenolysis. The resulting diamides are then either demethylated to produce the ...