4-氯-3-乙基-1-甲基-5-吡唑羧酸的合成研究
Synthesis of 4-chloro-3-ethyl-1-methyl-pyrazole-5-carboxylic acid
本文研究了从3-乙基-5-吡唑酸乙酯(1)出发,经过甲基化、氯化、水解酸化合成4-氯-1-甲基-3-乙基-5-吡唑羧酸(4)的方法。在甲基化反应中,以无毒的碳酸二甲酯替代剧毒品硫酸二甲酯,得到1-甲基-3-乙基-5-吡唑酸乙酯(2),中间体2经电化学氯化生成4-氯-3-乙基-1-甲基-5-吡唑酸乙酯(3),替代了文献硫酰氯的氯化方法,中间体3最后经水解酸化得到目标产物4-氯-3-乙基-1-甲基-5-吡唑甲酸(4)。整个工艺路线操作方法简便、反应条件温和,是一条环境友好的绿色合成工艺路线。
In this paper, the synthetic method of 4-chloro-3-ethyl-1-methyl-pyrazole-5- carboxylic acid (4) was reported from 3-ethyl-5-pyrazolecarboxylate (1) by methylation, chlorination, hydrolytic acidification. In methylation, 3-ethyl-1-methyl-5-pyrazolecarboxylate (2) was prepared by using atoxic dimethyl carbonate (DMC) instead of highly toxic dimethylsulfate. The intermediates 4-chloro-3-ethyl-1-methyl-5-pyrazolecarboxylate (3) was obtained by electrolytic chlorination instead of environmentally unfriendly reagents sulfuryl chloride. This method gets the advantages of simple work-up procedure, milder conditions, which is a green synthetic route.
郑瀚骁、刘波、王波、由君
有机化学工业精细化学工业电化学工业
甲基化反应电化学氯化唑虫酰胺吡螨胺4-氯-1-甲基-3-乙基-5-吡唑羧酸
methylationelectrochemical chlorinationtolfenpyradtebufenpyrad4-chloro-3-ethyl-1-methyl-pyrazole-5- carboxylic acid
郑瀚骁,刘波,王波,由君.4-氯-3-乙基-1-甲基-5-吡唑羧酸的合成研究[EB/OL].(2014-06-13)[2025-08-11].http://www.paper.edu.cn/releasepaper/content/201406-226.点此复制
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