新型杀螨剂吡螨胺的合成研究
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摘要
以草酸二乙酯、丁酮、水合肼和硫酸二甲酯为原料,经Claisen反应、Knorr环合法得到中间体3-乙基-1-甲基吡唑-5-羧酸乙酯(Ⅰ);(Ⅰ)经氯气氯化、水解、酰氯化和缩合反应,得到目标产物吡螨胺,总收率达40%(以草酸二乙酯计),产品纯度95%。采用的合成路线原料成本低,操作简便,适合工业化生产。
Ethyl,3-ethyl-1-methyl-5-pyrazolecarboxylate(Ⅰ) was synthesized through Claisen reaction and Knorr reaction from diethyl oxalate,2-butanone,hydrazine and dimethyl sulfate.Pyranica was prepared from(Ⅰ) by the chlorination,hydrolyzed reaction,acylation reaction and condensation reaction.The total yield for the synthesis of Pyranica was 40 % based on diethyl oxalate,and the purity of the product was 95 %.The synthesis route is suitable for industrial manufacture because of its low production cost and simple operation.
Ethyl,3-ethyl-1-methyl-5-pyrazolecarboxylate(Ⅰ) was synthesized through Claisen reaction and Knorr reaction from diethyl oxalate,2-butanone,hydrazine and dimethyl sulfate.Pyranica was prepared from(Ⅰ) by the chlorination,hydrolyzed reaction,acylation reaction and condensation reaction.The total yield for the synthesis of Pyranica was 40 % based on diethyl oxalate,and the purity of the product was 95 %.The synthesis route is suitable for industrial manufacture because of its low production cost and simple operation.
引文
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