摘要
[目的]选择性还原啶酰菌胺关键中间体2-硝基-4′-氯联苯废弃结晶母液中的原料邻氯硝基苯,回收中间体2-硝基-4′-氯联苯。[方法]以二氧化硫脲为还原剂,选择性将邻氯硝基苯还原为邻氯苯胺。[结果]最佳反应条件:邻氯硝基苯∶二氧化硫脲∶氢氧化钠的物质的量之比为1∶3.5∶8,反应温度为10℃,反应时间为3.5 h,2-硝基-4′-氯联苯最高回收率为78.95%。[结论]该方法不仅能选择性还原邻氯硝基苯,而且可高效回收2-硝基-4′-氯联苯,具有还原剂价廉易得、反应条件温和等优点。
[Aims]The study aims to selectively reduce ortho nitrochlorobenzene from the waste filtrate of2-nitro-4’-chlorobiphenyl crystallization and to recover 2-nitro-4’-chlorobiphenyl,a key intermediate of boscalid.[Methods]Selective reduction of ortho nitrochlorobenzene was conducted to obtain o-chloroaniline by using thiourea dioxide as reducing agent.[Results]The determined optimal condition for selective reduction was:molar ratio of ortho nitrochlorobenzene:thiourea dioxide:NaOH=1:3.5:8,the reaction temperature of 10℃and the reaction time of 3.5 h.The highest recovery rate of 2-nitro-4’-chlorobiphenyl was 78.95%.[Conclusions]The method not only can selectively reduce o-chloronitrobenzene,but also can efficiently recover 2-nitro-4’-chlorobiphenyl,and has the advantages of cheap reducing agent and mild reaction conditions.
作者
韩晓蕾
崔格
吕海军
郭庆春
张志虎
张越
HAN Xiao-lei;CUI Ge;LYU Hai-jun;GUO Qin-chun;ZHANG Zhi-hu;ZHANG Yue(School of Chemical and Pharmaceutical Engineering,Hebei University of Science and Technology,Shijiazhuang 050018,China;Hebei Lansen Biotechnology Co.,Ltd.,Jinzhou 052260,Hebei,China)
出处
《农药》
CAS
CSCD
北大核心
2019年第11期796-798,812,共4页
Agrochemicals
