水合肼还原制备2,4-二氯-5-炔丙氧基苯胺  

Preparation of 2,4-Dichloro-5-(ethynyloxy)benzenamine with Hydrazine Hydrate Reduction

作　　者：丁效明[1] 潘忠稳[1] 廖灵斌[1] 陶明山[1] 罗世宏[1] 

机构地区：[1]安徽大学化学化工学院,合肥230039

出　　处：《农药》2012年第8期573-574,589,共3页Agrochemicals

摘　　要：[目的]水合肼还原制备除草剂丙炔噁草酮的关键中间体2,4-二氯-5-炔丙氧基苯胺。[方法]以FeCl3/C为催化剂,采用80%水合肼还原2,4-二氯-5-炔丙氧基硝基苯,70℃下反应4 h。[结果]反应收率75%,含量98.3%,还获得了2,4-二氯-5-烯丙氧基苯胺、2,4-二氯-5-正丙氧基苯胺2种副产物杂质,采用IR、1H NMR表征了结构。[结论]2,4-二氯-5-炔丙氧基硝基苯可以被水合肼还原制备2,4-二氯-5-炔丙氧基苯胺,同时其部分不饱和碳碳键也可以在此条件下被还原加氢。[Aims] 2,4-Dichloro-5-（ethynyloxy）benzenamine, a key intermediate of oxadiargyl was prepared by hydrazine hydrate reduction. [Methods] 2,4-Dicbloro-5-（ethynyloxy）-4-nitrobenzene was reduced with 80% hydrazine hydrate in the presence of FeCl3/C catalyst at 70℃ for 4 h. [Results] The yield is 75% and purity is 98.3%. 2,4-Dichloro-5-（allyloxy） benzenamine and 2,4-dichloro-5-propoxybenzenamine as by-products were gained and the structure was confirmed by IR and ~H NMR. [Conclusions] It was found that 2,4-dichloro-5-（ethynyloxy）benzenamine could be prepared by reduction reaction of, 2,4-dichloro-5-（ethynyloxy）-4-nitrobenzene with hydrazine hydrate and some unsaturated carbon-carbon bond can also be reduced in this condition.

关 键 词：2 4-二氯-5-炔丙氧基苯胺 丙炔噁草酮 水合肼 还原 

分 类 号：TQ457.2[化学工程—农药化工]