3-乙氧基-4-{[3-(三氟甲基)苯基]氨基}环丁-3-烯-1,2-二酮的合成  

Synthesis of 3-ethoxy-4-(3-trifluoromethylphenylamino)-cyclobut-3-ene-1,2-dione

作　　者：白文辉 朱倩 刘娇 张少荟 高艳蓉 唐文强 BAI Wen-hui;ZHU Qian;LIU Jiao;ZHANG Shao-hui;GAO Yan-rong;TANG Wen-qiang(School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xi’an 712046,China;Collaborative Innovation Center of Green Manufacturing Technology for Traditional Chinese Medicine in Shaanxi Province,Xi’an 712046,China)

机构地区：[1]陕西国际商贸学院医药学院,陕西西安712046 [2]陕西省中药绿色制造技术协同创新中心,陕西西安712046

出　　处：《精细与专用化学品》2022年第1期42-45,共4页Fine and Specialty Chemicals

基　　金：陕西省大学生创新创业训练计划项目(S202113123043)。

摘　　要：以3-三氟甲基苯胺和方酸二乙酯等为原料,依次经过酯化和氨解反应合成了目标化合物3-乙氧基-4-{[3-(三氟甲基)苯基]氨基}环丁-3-烯-1,2-二酮。中间体及目标化合物结构经^(11)HNMR和MS表征,并考察了影响目标化合物收率的主要因素。确定氨解反应的适宜条件为:n(3-三氟甲基苯胺)∶n(方酸二乙酯)=1.1∶1;反应溶剂为二氯甲烷,反应时间为8h。在此条件下,目标化合物的收率为73%(以方酸二乙酯计)。The synthesis of a square amide monoethyl ester 3-ethoxy-4-((3-(trifluoromethyl)phenyl)amino)cyclobut-3-ene-1,2-dione was reported.The target compound was obtained by esterification and ammonolysis using square acid and 3-trifluoromethylphenylamine as raw material.The structures of intermediates and products were characterized by ^(1)HNMR and MS.The main factors affecting the yield of the product were investigated.The optimum conditions of the ammonolysis reaction were as follows: The ratio of material n(3-trifluoromethylaniline)∶n(diethyl squarate) = 1.1∶1;the reaction solvent was dichloromethane;the reaction time was 8 h.Under this condition, the yield of the target product was 73%(the yield was calculated based on diethyl square acid).

关 键 词：方酰胺 氨解反应 工艺研究 合成 

分 类 号：TQ463[化学工程—制药化工]