以乙醇为溶剂,冰醋酸为催化剂,4-氨基-5-(1-苯基-3-甲基-5-氯吡唑)-1,2,4-三唑-3-硫酮(1)与芳醛经缩合反应合成了7个新型的4-取代苯次甲亚胺-5-(1-苯基-3-甲基-5-氯吡唑)-4H-1,2,4-三唑-3-硫酮(3a~3g),收率66%~74%,其结构经^1H NMR,IR及元素分析表征。合成4-(苯次甲亚胺)-5-(1-苯基-3-甲基-5-氯吡唑)-2H-1,2,4-三唑-3-硫酮(3a)的最佳反应条件为:以乙醇为溶剂,乙酸为催化剂,1 10 mmol,n(苯甲醛)∶n(1)=1.2,于75℃反应3 h,产率74%。
Seven novel 4-( substitutedbenzylideneamino)-5-( 5-chloro-3-methyl-1-phenyl-1H-pyrazol-4-yl)-2H-1,2,4-triazole-3( 4H)-thiones( 3a ~ 3g) in yield of 66% ~ 74% were synthesized by condensation reaction of 4-amino-5-( 5-chloro-3-methyl-1-phenyl-1H-pyrazol-4-yl)-2H-1,2,4-triazole-3( 4H)-thione( 1) with aromatic aldehyde using acetic acid as the catalyst in ethanol. The structures were characterized by ^1H NMR,IR and elemental analysis. The yield of 4-( benzylideneamino)-5-( 5-chloro-3-methyl-1-phenyl-1H-pyrazol-4-yl)-2H-1,2,4-triazole-3( 4H)-thione( 3a) was 74% under the optimal reaction conditions[ethanol was solvent,acetic acid was catalyst,1 was 10 mmol,n( benzaldehyde) ∶ n( 1) was 1. 2,at 75 ℃ for 3 h].