Long-chained amphiphiles containing a sulfonyl group accompanied by azobenzene moieties and heterocyclic rings (thiazolyl or pyrimidinyl) were obtained. It was found that the derivatives of sulfathiazole (I and III) were more effective in monolayer formation as compared with sulfadiazine ones (II and IV) and their pi-sigma isotherms were characterized by a high collapse pressure, at sigma reaching 0.24-0.25 nm(2). The transfer ratio of the monolayer onto silver-coated glass slides was in the range 0.95-0.98. The average thickness of the monolayer transferred onto the slides (determined by surface plasmon resonance) amounted to 3.05-3.25 nm, depending on the length of the amphiphile hydrophobic chain. The amphiphiles in question, with a donor-acceptor molecular structure separated by pi-electron system, showed nonlinear optical properties with the first hyperpolarizability values being 3.6-3.8 times that of p-nitroaniline.