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[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。
[Objective] Diaryl ethers are important pesticide intermediates for the synthesis of many important insecticides, such as some pyrethroids, fungicides such as ether azoles and other pesticides. 3,4’-dichlorodiphenyl ether and 3-methyl-diphenyl ether are the key intermediates of ether azole and fenvalerate respectively. Traditionally, copper powder has been used as a catalyst for its low efficiency and selectivity. To this end, Two kinds of diaryl ether intermediates were optimized and improved. [Method] Commercial copper powder and self - made highly dispersed copper were used as catalysts to optimize the synthesis of two kinds of diaryl ether intermediates by solvent, reaction molar ratio, reaction temperature and reaction time respectively. [Result] The selectivity of 3,4’-dichlorodiphenyl ether reached 86.7% and the yield was 82.2%. The yield of 3-methylenediphenyl ether was 96.8%. [Conclusion] The experimental results show that the catalytic activity and selectivity of highly dispersed copper are better than the traditional Ullmann reaction catalyst.