N′-叔丁基-3,5-二氯苯甲酰基-N-吡唑酰基肼的合成工艺研究

Study on the Synthesis Technology of N′-Tert-butyl-3,5-dichlorobenzoyl-N-pyrazolylhydrazine Compounds

N′-叔丁基-3,5-二氯苯甲酰基-N-吡唑酰基肼在5μg·mL^(-1)浓度时对小菜蛾(Plutella xyllostell)致死率达到100%,1μg·mL^(-1)浓度时为60%,活性是虫酰肼(Tebufenozide)的5倍。以4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酸、叔丁基肼、3,5-二氯苯甲酸为原料合成了N′-叔丁基-3,5-二氯苯甲酰基-N-吡唑酰基肼。用~1 H NMR对产品结构进行了确定,找到了合成中间体和目标产物的最佳工艺条件,为产品工业化生产提供了指导。

The N′-tert-butyl-N-4-chloropyrazolylhydrazine compounds have 100% mortality in 5μg·mL^(-1) and 60% mortality in 1μg·mL^(-1) to Plutella xyllostell,which is 5 times as effective as the Tebufenozide.N′-Tert-butyl-3,5-dichlorobenzoyl-N-pyrazolylhydrazine was prepared by the reaction of 4-chloro-3-ethyl-1-methyl-1H-pyrazole-5-carboxylic acid,tert-butyl hydrazine and 3,5-dichlorobenzoic acid.The structure of product was characterized by ~1 H NMR.The optimum conditions of preparing intermediate and target compound were obtained and will provide guidance for the industrial production.