杀虫剂chlorantraniliprole合成新方法

New Method for Synthesis of Chlorantraniliprole Insecticide

改进杀虫剂chlorantraniliprole合成方法,以3-溴-1-(3-氯-2-吡啶基)-1H-吡唑-5-羧酸、2-氨基-5-氯-3-甲基苯甲酸为原料,使用光气/3-甲基吡啶体系催化进行合环反应,最后与一甲胺反应生成目标化合物chlorantraniliprole,其结构经过1H NMR确证。在最佳的光气用量、合环反应温度条件下的总收率为81.4%,高效液相纯度为96.4%。改进后的合成方法反应条件温和,反应时间短,后处理简单,三废较少;原料廉价易得,经济可行性高。

The synthesis method of chlorantraniliprole was improved.Chlorantraniliprole was synthesized from 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid and 2-amino-5-chloro-3-methylbenzoic acid.The phosgene/3-methylpyridine system was used to catalyze the cyclization.Then it reacted with monomethylamine to produce the chlorantraniliprole.The structure of the target compound was confirmed by 1H NMR.The total yield and HPLC purity were 81.4%and 96.4%at the optimum phosgene dosage and cyclic reaction temperature respectively.The improved synthesis method has mild reaction conditions,less reaction time,simple post-processing and less waste.Raw materials are cheap and easy to obtain with high economic feasibility.