Abstract: Aryloxyphcnylthiophosphonyl hydrazidc (Ⅰ) has been synthesized by the reaction of aryloxyphcnylthiophospllcny! hloridc with excess of 50% hydrazinehydratc and NN'-bis [aryloxyphenylthiophosphoyl] hydrazidc (Ⅱ) was isolated in some of these reaction.The Diastereomer of optically active hydrazone were obtained by the reaction of (Ⅰ)with (-) mcnthonc.One of the optical isomcr of ethoxyphenyl-thiophosphonyl(-)menthonc hydrazone was chromatographed with the silica gel co-lumn,IR,¹H NMRand Mass Spectra of the title compounds were discussed.