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Aim: This study includes the synthesis and diagnosis of the 3,3’-(disulfanediylbis (methylene))bis(1-(4-bromophenyl)-4-(4-chlorophenyl)azetidin-2-one)2d. Methods: This compound was ready through the reaction of the 3,3’-disulfanediyldipropionic acid with the appropriate 4-bromo-N-(4-chlorobenzylidene) aniline 1d. Results: The structure of those azetidin-2-one was diagnosed on the premise of the spectral data: Infrared (IR); proton nuclear magnetic resonance (¹H-NMR); carbon-13 NMR (13C-NMR); and mass. Conclusion: This work approved the synthesis of 3,3’-(disulfanediylbis(methylene))bis(1-(4-bromophenyl)-4-(4-chlorophenyl)azetidin-2-one) compound from 3,3’-disulfanediyldipropionic acid and appropriate Schiff’s bases using POCl3 and Et3N in CH2Cl2 under N2 atmosphere and characterization of these compound by IR, mass, (2D-NMR experiments) ¹H-NMR, and 13C-NMR spectra. [ABSTRACT FROM AUTHOR]