Condensation of propane-1,3-diamine or benzene-1,4-diamine with 2-phenyl-1,2,3-triazole-4- carboxaldehyde give a series of new bis-Schiff bases 3 and 4, which were then reacted with α-chloro-oximes to afford a bis-1,2,4-oxadiazoline derivatives 6a～6f and 7a～7f by 1,3-dipolar cycloaddition. The new compounds were characterized by elemental analysis, IR, 1H NMR, MS techniques and X-ray diffraction analysis. The crystal of the compound 6e belongs to monoclinic, space group C2/c with cell parameter a＝3.5134(8) nm, b＝0.50575(11) nm, c＝2.0598(5) nm, α＝90°, β＝102.02(8)°, γ＝90°, Mr＝756.81, V＝3.5798(14) nm3, Dc＝1.404 g/cm3, Z＝4, F(000)＝1576, μ＝0.095 mm－1, R＝0.0787 and wR＝0.2093.

Key words: bis-Schiff base, crystal structure, 1,3-dipolar cycloaddition, bis- 1,2,4-oxadiazoline derivatives, 2-phenyl-1,2,3-triazole-4-carboxaldehyde