摘要
以氰基乙酰胺为原料,经过肟化、乙基化、氨解、溴代、环合、碱性水解六步反应制得(Z)-2-(5-氨基-1,2,4-噻二唑-3-基)-2-乙氧基亚胺基乙酸(ATDE),总收率37.8%。通过MS和1HNMR对目标产物及各步反应中间体的结构进行了表征。改进了2-氰基-2-乙氧亚胺基乙酰胺的合成工艺,确定了最优工艺条件:n(氰基乙酰胺)∶n(亚硝酸钠)∶n(酸)∶n(硫酸二乙酯)=1∶1.5∶2∶1.2,采用盐酸,反应温度48℃,反应时间3h,收率提高至89.1%。对于水解过程,最优工艺条件为:采用氢氧化钾,反应温度55℃,反应时间7h。
2-Cyanoacetamide was used as the starting material,through oximation,alkylation,aminolysis,bromination,cyclization,hydrolysis to obtain (Z)-2-(5-amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetic acid(ATDE).The total product yield was 37.8%.The structures of the target products and its intermediates were characterized by MS and 1H NMR spectra.The synthesis process of 2-cyano-2-ethoxyiminoacetamide was improved,and the optimal process conditions were determined:n (cyanoacetamide)∶ n (sodium nitrite)∶ n (acid)∶ n (diethyl sulfate)=1 ∶1.5 ∶2 ∶1.2,under the condition of hydrochloric acid,reaction temperature 48 ℃,reaction for 3 h,the yield was increased to 89.1%.In the process of hydrolysis,the optimum reaction were as follows:Potassium hydroxide provides an alkaline environment,reaction temperature 55 ℃,and reaction for 7 h.
作者
王付刚
薛峰
曹辉
居沈贵
WANG Fu-gang;XUE Feng;CAO Hui;JU Shen-gui(College of Chemical Engineering,Nanjing Tech University,Nanjing 211816,China)
出处
《应用化工》
CAS
CSCD
北大核心
2019年第10期2280-2283,共4页
Applied Chemical Industry
基金
国家自然科学基金(U1407122)
江苏省创新工程(SJCX18_0338)
