唑蚜威合成工艺研究

Study on the Synthesis Technology of Triazamate

探索可工业化生产唑蚜威的合成工艺.结合实际生产情况,以氨基硫脲、三甲基乙酰氯、氯乙酸乙酯、N,N-二甲基氨基甲酰氯为原料合成唑蚜威.试验三唑环合成的碱性条件,烷基化的碱性条件,N-取代酰化的催化剂、缚酸剂、后处理条件,改进了1,2,4-三唑杂环合成、S-烷基化、N-取代酰化的合成工艺条件.并通过测定红外光谱、核磁共振氢谱、熔点,对唑蚜威进行结构表征,得到总收率60.87%、产品HPLC纯度96.23%(质量分数)的唑蚜威合成新工艺.

To explore the synthesis process of pyrimicard which can be industrialized,combined with the actual production,synthesis of triazamate with thiosemicarbazide,trimethylacetyl chloride,ethyl chloroacetate,N,N-dimethylcarbamoyl chloride,etc.Basic conditions for the synthesis of triazole ring,the alkylated alkaline condition,N-substituted acylation catalyst,acid binding agent,post-treatment condition were tested.The synthesis process of 1,2,4-triazole heterocyclic ring synthesis,S-alkylation and N-substituted acylation was improved.The structure of triazamate was characterized by measuring infrared spectrum,nuclear magnetic resonance spectrum and melting point.The total yield of the product was 60.87%,and the HPLC purity of the product was 96.23%.