Novel N,N'-bisethoxyethane[12]amideferrocenophane has been synthesized by a condensation reaction and characterized by H-1 NMR and mass spectrum. The anion recognition properties of the compound are evaluated via H-1 NMR, FT-IR, and electrochemical measurement. It is found that N,N'-bisethoxyethane[12]amideferrocenophane exhibits remarkable electrochemical response to H2PO4- anion in CH2O2 or CH3CN solution, and response to anions can also be observed in CH3CN solution containing up to 15% water. Binding constants between the compound and HSO4- in different solutions have been determined by UV-vis spectrum titration experiments. The results indicate that the compound shows a selective recognition trend of H2PO4- > HSO4- (F-) > Br-.