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[目的]制备氯虫酰胺的重要中间体3-溴-1-(3-氯-2-吡啶基)-1H-吡唑-5-甲酸。[方法]以2,3-二氯吡啶为原料,经肼解、环合、溴化、氧化、水解制得3-溴-1-(3-氯-2-吡啶基)-1H-吡唑-5-甲酸。[结果]在优化的条件下,反应总收率为41.87%(以2,3-二氯吡啶计),含量为98.5%,其结构经1H NMR分析确认。[结论]该工艺简单经济,条件温和,适合工业化生产。
[Objective] To prepare 3-bromo-1- (3-chloro-2-pyridyl) -1H-pyrazole-5-carboxylic acid, an important intermediate of chlorantraniliprole. [Method] 2,3-dichloropyridine was used as starting material to prepare 3-bromo-1- (3-chloro-2-pyridyl) -1H-pyrazole by hydrazinolysis, cyclization, -5-carboxylic acid. [Result] Under the optimized conditions, the total yield of the reaction was 41.87% (calculated as 2,3 - dichloropyridine), the content was 98.5%. Its structure was confirmed by 1H NMR analysis. [Conclusion] The process is simple and economical, mild conditions, suitable for industrial production.