anti-Chlorophenylglyoxime(CPGH2) has been synthesized by chlorination of anti-phenylglyoxime. The reaction of CPGH2 with P-chloroaniline, o-chloraniline and m-chloroaniline in ethanol between -10-degrees-C and -15-degrees-C gives unsymmetrical vic-dioximes, namely, p-chloroanilinophenylglyoxime (p-CAPGH2), o-chloroanilinophenylglyoxime (o-CAPGH2), m-chloroanilino-phenylglyoxime (m-CAPGH2). H-1-NMR, mass, IR spectra and elemental analyses data are given.