Three acylhydrazone-based compounds were designed as novel neutral sensors for anions, and synthesized by simple steps in good yields. Their anion recognition properties were studied by UV-vis and (1) H-NMR spectroscopy. The results showed that the receptors 1, 2, and 3 all had a better selectivity for F(-) and CH(3)COO(-), but no evident binding with Cl(-), Br(-), I(-), NO(3)(-), H(2)PO(4)(-), or HSO(4)(-). The results indicated that anion recognition was achieved via convergent hydrogen bond interactions from acylhydrazone functionality on the side arms. The UV-vis data indicated that a 1: 1 stoichiometry complex was formed between compounds 1, 2, or 3 and anions. The binding and selectivity were also tuned by the change of the place of the nitro group attached to the phenyl. Moreover, receptor 3 can act as the colorimetric sensor for such anions as F(-) and CH(3)COO(-), and the recognition mechanism and binding mode were discussed.