Synthesis Of Fe-groups Transition Metal Complex

Starting from o-phenylenediamine,4-Nitro-o-phenylenediamine,dimethyl malonic acid,oxalyl chloride,diethyl oxalate and Anhydrous metal chlorides etc,five synthetic routes were designed to synthetic some more stable macrocyclic ligands,totally,2 complex catalysts with transition metal as the central atom and 8 intermediates were synthesized.The influence of the reaction temperature,reaction time,rate of feeding,mode of feeding,control of anhydrous condition as well as the choice of solvent on the formation of product was studied and the synthetic routes were optimized.The intermediates and final product were characterized with NMR and MS.4-Nitro-o-phenylenediamine can react with Ethyl oxalyl monochloride and o-phenylenediamine using THF and ethanol as the solvents and target product was formed.The product can be conveniently separated from the reaction solution and yields 78.5%,this reaction conditions is mild and easy to control.12H4L and 2F-13H4L was produced by amine ester hydrolysis reaction,avoiding the generation of 6H2L.Two kinds of open loop products were produced by 8-aminoquinoline and chloride,and both yield more than 86%.