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2种二芳醚农药中间体的合成
引用本文:杨秋月,王芳,孙宁宁,姜鹏.2种二芳醚农药中间体的合成[J].农药,2012,51(1):16-18,65.
作者姓名:杨秋月  王芳  孙宁宁  姜鹏
作者单位:1. 沈阳化工研究院有限公司,沈阳110021;沈阳化工大学,沈阳110042
2. 沈阳化工研究院有限公司,沈阳,110021
基金项目:国家"十二·五"科技支撑计划项目,国家重点基础研究发展计划(973计划)项目
摘    要:目的]二芳醚是重要的农药中间体,用于合成多种重要的杀虫剂,如一些拟除虫菊酯、杀菌剂如醚唑等农药。3,4’-二氯二苯醚和3-甲基二苯醚分别是醚唑和戊菊酯的关键中间体,传统上采用铜粉为催化剂合成效率和选择性欠佳,为此,对2种二芳醚中间体合成进行优化和改进。方法]采用商用铜粉和自制高分散铜为催化剂,分别对溶剂、反应摩尔比、反应温度、反应时间进行优化合成2种二芳醚中间体。结果]3,4’-二氯二苯醚的选择性达86.7%,收率为82.2%;3-甲基二苯醚的收率为96.8%。结论]实验结果显示高分散铜的催化活性和选择性都好于传统Ullmann反应催化剂。

关 键 词:高分散铜  3  4’-二氯二苯醚  3-甲基二苯醚  合成

Syntheses of Two Diaryl Ethers for Pesticide Intermediates
YANG Qiu-yue , WANG Fang , SUN Ning-ning , JIANG Peng.Syntheses of Two Diaryl Ethers for Pesticide Intermediates[J].Pesticides,2012,51(1):16-18,65.
Authors:YANG Qiu-yue  WANG Fang  SUN Ning-ning  JIANG Peng
Affiliation:1 (1.Shenyang Research Institute of Chemical Industry Co.,Ltd.,Shenyang 110021,China; 2.Shenyang University of Chemical Technology,Shenyang 110042,China)
Abstract:Diaryl ether are an important intermediate of the pesticide,which are widely used in synthesis of insecticides such as pyrethroids,and fungicides such as dienoconazole.3,4’-Dichlorodiphenyl ether and 3-methyl diphenyl ether are key intermediates of dienoconazole and fenvalerate,respectively.Traditionally,synthetic effeciency and selectivity are poorer when powder Cu was used as catalyst,so in this paper,the syntheses of the two diaryl ethers were optimized and improved.Methods] Commercial available powder Cu and high-dispersed Cu made by ourself are used as catalysts,a series of synthetic conditions such as solvents,various molar ratio of substrates,reaction temperature,reaction time,etc.are observed and optimized to synthesize these two diaryl ether intermediates.Results] the selectivity of 3,4’-dichlorodiphenyl ether was up to 86.7% with yield of 82.2%,while the yield(96.8%) of 3-methyl diphenyl ether was obtained.Conclusions] the experiment results showed that the catalytic activity and selectivity of high-dispersed copper are both better than that of traditional Ullmann reaction catalyst.
Keywords:high-dispersed copper  3  4’-dichlorodiphenyl ether  3-methyl diphenyl ether  synthesis
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