由 β-苯丙烯酰氯与取代苯肼的缩合反应合成了芳基取代的 α,β-不饱和酰肼化合物 ,进而利用相转移催化剂 4-羟基 - 2 ,2 ,6 ,6 -四甲基 - 1 -哌啶基氧自由基以及 Galvinoxyl自由基对其进行了相转移催化脱氢 ,合成了 8种芳基取代的 α,β-不饱和酰基偶氮新型化合物 ,其结构经元素分析、IR和 1 H NMR证实。并讨论了可能的反应机理。 Aromatic - substituted α, β - unsaturated hydrazide compounds were synthesized by the condensation reaction of β - phenylpropenoyl chloride and substituted phenylhydrazine. The phase transfer catalyst 4 - hydroxy - 2,2,6,6 - tetramethyl - 1 - piperidinyloxy free radical and Galvinoxyl free radical were used to catalyze dehydrogenation. Eight kinds of aryl-substituted α, β-unsaturated acylazo compounds were synthesized and their structures were characterized by elemental analysis, IR and 1 H NMR confirmed. The possible reaction mechanism was discussed.