A combination of crosslinked poly(4-vinylpyridinium)chloride [P-4-H]Cl (I) and sodium nitrite or quaternized crosslinked poly(N-methyl-4-vinylpyridinium)nitrite [P-4-Me]NO2 (II) was used as effective nitrosating agents for the N-nitrosation of secondary amines under mild and heterogeneous conditions in moderate to excellent yields. The spent polymeric reagents can usually be removed quantitatively and regenerated. (c) 2007 Wiley Periodicals, Inc.