N-(2-甲基)苯基羟胺的合成新工艺  

New Processing for N-2-Methylphenylhydroxyamine

作　　者：闻东亮 刘志山 孙军利 刘彦涛 郑先福[2] 

机构地区：[1]郑州郑氏化工产品有限公司,郑州450008 [2]河南农业大学理学院,郑州450008

出　　处：《农药》2015年第12期879-882,共4页Agrochemicals

基　　金：河南省攻关项目(132102310251)

摘　　要：[目的]N-(2-甲基)苯基羟胺是一种重要农药中间体,用选择性还原方法进行合成。[方法]以邻硝基甲苯为主要原料,经Raney Ni-水合肼还原制备N-(2-甲基)苯基羟胺。[结果]在优化的反应条件下,N-(2-甲基)苯基羟胺的反应收率为78.5%。加入适量SiO^2颗粒后,反应收率可达90.2%。补加适量催化剂后,Raney Ni可套用1次。由于N-(2-甲基苯基)羟胺在空气中不稳定,尝试了进一步与氯甲酸甲酯反应制备N-羟基-N-2-甲苯氨基甲酸甲酯,2步总收率85.7%(含量为98.2%),其结构经氢谱核磁分析确证。[结论]N-(2-甲基)苯基羟胺合成工艺具有生产成本低、收率高和易于工业化生产等优点。[Aims] As an important intermediate of pesticides, N-2-methylphenylhydroxyamine was synthesized by method of selective reduction. [Methods] A synthesis process of N-2-methylphenhyldroxyamine was studied by reducing o-nitrotoluene using N2H4-H2O under Raney Ni condition. [Results] Under the optimal condition, the yield was 78.5%. It could be increased to 90.2% by adding the certain quantity of SiO^2. After a small amount of Raney Ni, it can be used again. As it is unstable in the air, the N-2-methylphenylhydroxylamine was further converted into corresponding carbamate by reacting with methyl chloroformate. The total yield was 85.7% and the structure was confirmed by1 H NMR. [Conclusions] The process showed low cost and high yield, and is suitable for industrial production.

关 键 词：邻硝基甲苯 N-(2-甲基苯基)羟胺 合成 

分 类 号：TQ455.4[化学工程—农药化工]