甲氧胺盐酸盐的合成工艺  

STUDY ON THE SYNTHETIC PROCESS OF METHOXAMINE HYDROCHLORIDE

作　　者：杨士伟 朱金苗[1,2] 郑斌 王小红[1] 毕文杰 张雪燕 Yang Shiwei;Zhu Jinmiao;Zheng Bin;Wang Xiaohong;Bi Wenjie;Zhang Xueyan(College of Chemical and Pharmaceutical Engineering,Hefei Normal University,Hefei 230601,Anhui,China;Laboratory of Development and Function of Medicinal and Food Resources in Anhui Province,Hefei 230601,Anhui,China)

机构地区：[1]合肥师范学院化学与制药工程学院,安徽合肥230601 [2]安徽省药食同源资源与功能开发实验室,安徽合肥230601

出　　处：《精细石油化工》2024年第6期56-59,共4页Speciality Petrochemicals

基　　金：2024年安徽省高校科学研究重点项目(2024AH051591);安徽省药食同源资源开发功能实验室开放基金项目(YSTY2022020)。

摘　　要：报道了以盐酸羟胺为原料的甲氧胺盐酸盐合成新工艺。优化合成工艺条件为:1)盐酸羟胺用量20 g,n(盐酸羟胺)∶n(碳酸钾)=2∶1,V(乙酸乙酯)=150 mL,V(50%乙醇)=150 mL,反应温度80℃,反应时间5.0 h,得到乙酰羟胺(Ⅰ);2)n(化合物Ⅰ)∶n(硫酸二甲酯)=1.68∶1,反应温度0~25℃,反应时间4.0 h,150 mL 50%NaOH-乙醇溶液,得到乙酰甲氧胺(Ⅱ);3)以水为溶剂,n(化合物Ⅱ)=0.5612 mol,V(H_(2)SO_(4))=50 mL,反应温度70℃,反应时间4.0 h,得到甲氧胺盐酸盐。三步反应的总收率为74.47%。A new process for the synthesis of methoxyamine hydrochloride using hydroxylamine hydrochloride as raw material was studied.The optimal synthesis process conditions are:1)n(hydroxylamine hydrochloride)∶n(potassium carbonate)=2∶1,V(ethyl acetate)=150 mL,V(50%ethanol)=150 mL,reaction temperature of 80℃,and reaction time of 5.0 h,acetylated hydroxylamine(Ⅰ)was obtained;2)n(Ⅰ)∶n(dimethyl sulfate)=1.68∶1,reaction temperature of 025℃,reaction time of 4.0 h,V(50%NaOH-ethanol)=150 mL,acetylmethoxyamine(Ⅱ)was obtained;3)using water as the reaction solvent,n(Ⅱ)=0.5612 mol,V(H_(2)SO_(4))=50 mL,reaction temperature of 70℃,reaction time of 4.0 h,methoxyamine hydrochloride was obtained.The total yield of methoxyamine hydrochloride obtained through a three-step reaction is 74.47%.

关 键 词：盐酸羟胺 硫酸二甲酯 甲氧胺盐酸盐 乙酰甲氧胺 循环套用 

分 类 号：TQ463[化学工程—制药化工]