A combination of cross-linked poly(4-vinylpridininium) chloride [P-4-H] Cl, [II], and sodium nitrite or quaternized cross-linked poly(N-methyl-4-vinylpyridinum) nitrite [P-4-Me] NO2, [IV], was used as effective nitrosating agents for the N-nitrosation of secondary amines under solvent-free conditions in high yields. The spent polymeric reagents can usually be removed quantitatively and regenerated. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 114: 2134-2138,2009