Abstract The synthesis of “reactive”(ie aminoacylated) fluoroaliphatic diamines [H 2 N (CH 2) 3 C ( O) NHCH 2 CH 2 (CF 2) n CH 2 CH 2 NHC ( O)(CH 2) 3 NH 2; n= 4, 8] has been accomplished through the use of peptide blocking group and coupling techniques. Also, the synthetic route to these diamines and their dihydrobromide salts has been improved over that of a recently published procedure.