Diethyl 2,2´ [1,2 phenylenebis(aminomethylidene)]bis(3 oxo 3 polyfluoroalkylpropion ates) were synthesized by the condensation of a double excess of ethyl 2 ethoxymethylidene 3 oxo 3 polyfluoroalkylpropionates with o phenylenediamine. The use of equimolar ratios of the starting reactants affords ethyl 2 [(2 aminophenyl)aminomethylidene] 3 oxo 3 polyfluoroalkylpropionates from which nonsymmetric biscondensation products were syn thesized by the reaction with related reactants containing different polyfluoroalkyl substituent. The copper(II), nickel(II), and cobalt(II) complexes were obtained on the basis of new ligands.Interest in synthesis of metal complexes based on azomethine compounds is caused by their catalytic activity in polymerization reactions 1-3 and magnetic 4-7 and luminescence 8,9 properties. Non fluorinated 2 ethoxy methylidene 1,3 dicarbonyl compounds in reactions with 1,2 diamines form biscondensation products at the ethoxymethylidene moiety 10-12 and related metal com plexes. 13-16 It is possible to obtain monocondensation products 17-19 from which symmetric and asymmetric ligands 20 were synthesized, including the macrocyclic ligands 15,17-20 used in the synthesis of the metallocomplex compounds. 17-20 Schiff bases obtained by transformations of 2 ethoxymethylidene 3 oxo 3 fluoroalkylpropionates with different diamines can also serve as organic mol ecules forming the ligand shell. It is known 21 that the introduction of the fluorine atom into organic molecules changes their physicochemical properties, reactivity, bio logical activity and other characteristics caused by the presence of electronegative fluorine atoms and important in practical and theoretical aspects. However, published data on the participation of polyfluorinated analogs in similar polycondensation reactions are lacking.In the present work, we studied the reactions of ethyl 2 ethoxymethylidene 3 oxo 3 polyfluoroalkylpropion ates 1 with o phenylenediamine with the purpose to syn thesize new ligands and analyzed a possibility of the prepa ration of related metallocomplex compounds with a series of transition metals.It was found that the reaction of compounds 1a-c with 1 equiv. of o phenylenediamine in diethyl ether at room temperature afforded the monoadducts, viz., ethyl 2 [(2 aminophenyl)aminomethylidene] 3 fluoroalkyl 3 oxopropionates 2a-с, as a result of the nucleophilic attack of the amino group at the ethoxymethylidene moiety (Scheme 1). The use of a double excess of esters 1a-c results in the formation of symmetric products 3a-c due to the condensation of two molecules of ester 1a-c with one diamine molecule.Monosubstitution products 2а-c contain free NH 2 groups, which makes it possible to carry out their further transformations. The condensation of compounds 2а,с with the corresponding substrates 1a,b (see Scheme 1)