In this research we have synthesized a new macrocyclic Schiff base (II) containing nitrogen- oxygen donor atoms which was designed and synthesized by reaction of: 1,4– bis (6',6'- methoxy -3- formyl phenyl)-1,4- dioxa butane (I). Identification of this macrocyclic schiff base: (II) 1,16- Diaza–[3,6;11,14-di (6',6'- methoxy phenyl)]-7,10,19,22 - tetraoxa cyclo tetra icozane-15,1dien was determined by (LC-MS) and spectroscopy (IR). The liquid- liquid extraction of metal such as Zn2+, Pb2+ and Ni2+ from aqueous phase to organic phase which doesn't in water. The effect of chloroform and dichloromethane as organic solvents over the metal extractions was investigated at 25± 0.10C by using atomic absorption Spectrometer and extraction percentage was calculated.