第 50 卷第 5 期Vol. 50 No. 5
2020 年 10 月Oct 2020

所属栏目:农药及中间体

环保型杀菌剂啶酰菌胺的合成
尚 宇 ,李 飞,郭亚飞 (陕西省环境监测中心站,陕西 西安 710054)
摘 要:研究了一种合成环保型杀菌剂啶酰菌胺的方法,并优化其合成工艺。以邻氯硝基苯和4-氯苯硼酸为原料,经过Suzuki偶联、还原、缩合3步反应合成啶酰菌胺。在优化的反应条件下,3步总收率≥43%(以邻氯硝基苯计),产物纯度98%;产物结构经IR、1H NMR、MS确证。第1步Suzuki偶联反应中,优化的反应条件是无水碳酸钾作碱,催化剂四(三苯基膦)钯的用量为15%(以邻氯硝基苯计)。第2步还原反应温度为50 ℃。该工艺简单经济,条件温和,绿色环保。
关键词:环保;杀菌剂;啶酰菌胺;合成
中图分类号:S482.2  文献标识码:A  文章编号:1009-9212(2020)05-0012-04
Green Synthesis of A New Environmental Friendly Fungicide Boscalid
SHANG Yu, LI Fei, GUO Ya-fei (Shaanxi Environmental Monitoring Center, Xi'an 710054, China)
Abstract:A method for the synthesis of fungicide boscalid, a new environmental friendly bactericide was studied and the synthetic process was further optimized. Boscalid was prepared using 1-chloro-2-nitrobenzene and 4-chlorophenylboronic acid as starting materials through a series of reactions including Suzuki coupling reaction, reduction and condensation. Under the optimal reaction conditions, the total yield of boscalid was over 43% based on 1-chloro-2-nitrobenzene with a purity of 98%. The structure was confirmed by IR, 1H NMR, MS. In the first step, K2CO3 being used as alkali, 15% of catalyst Pd(PPh3)4 based on 1-chloro-2-nitrobenzen was used as the optimized condition. The optimal reaction temperature of the second reduction reaction is 50 ℃. This process is simple, mild, economical, and environmental friendly.
Key words:environmental friendly; boscalid; fungicide; synthesis
作者简介:尚 宇(1983—),男,辽宁抚顺人,工程师,主要从事环境监测工作(E-mail:523588666@qq.com)。
收稿日期:2020-07-31