1-(4-氟苯基)-2-(1H-1,2,4-三唑-1-基)乙酮的合成  

Synthesis of 1-(4-Fluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethan-1-one

作　　者：杨阳 包禧艳 雷宁 门靖 薛美玲 YANG Yang;BAO Xi-yan;LEI Ning;MEN Jing;XUE Mei-ling(Xi'an Manareco New Material Co.,Ltd.,Xi'an 710077,China;Xi'an Renalysis Medical Technology Co.,Ltd.,Xi'an 710304,China;Hanjiang-to-Weihe river valley water diversion project construction Co.,Ltd.,Xi'an 710086,China;Xi'an WanLong Pharmaceutical Co.,Ltd.,Xi'an 710119,China;Ginwa Enterprise(Group)INC.Xi'an Ginwa Pharmaceutical Factory,Xi'an 710075,China)

机构地区：[1]西安瑞联新材料股份有限公司,陕西西安710077 [2]西安乐析医疗科技有限公司,陕西西安710304 [3]陕西省引汉济渭工程建设有限公司,陕西西安710086 [4]西安万隆制药股份有限公司,陕西西安710119 [5]金花企业(集团)股份有限公司西安金花制药厂,陕西西安710075

出　　处：《精细化工中间体》2023年第6期17-19,59,共4页Fine Chemical Intermediates

摘　　要：在碳酸钾碱性条件下,以2-溴-1-(4-氟-苯基)乙酮(2)为起始原料,与1,2,4-三唑(3)发生亲核取代反应,合成得到目标化合物1-(4-氟苯基)-2-(1H-1,2,4-三唑-1-基)乙酮(1a)和副产物1-(4-氟苯基)-2-(1H-1,2,4-三唑-4-基)乙酮(1b),产物结构经^(1)HNMR和ESI-MS表征确证。优化的反应条件为:物料比n(3):n(2)=1.3:1.0、反应溶剂为乙腈、反应温度为25℃、反应时间4h,在该条件下,产物的收率达62.6%(以2计)。1-(4-Fluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethan-1-one(la)and the by-product 1-(4-fluorophenyl)-2-(1H-1,2,4-triazol-4-yl)ethanone(1b)was synthesized by the nucleophilic substitution of 2-bromo-1-(4-fluorophenyl)ethan-1-one(2)and 4H-1,2,4-triazole(3)under the alkaline condition of potassium carbonate.The structure of the product was characterized by^(1)H NMR and mass spectrometry(ESI-MS).The optimum reaction conditions were as followings:material mole ratio was n(3):n(2)=1.3:1.0,the reaction solvent was acetonitrile,the reaction temperature was 25 and the reaction time was 4 h.Under this reaction conditions,the yield of the product was 62.6%(calculated based on 2).

关 键 词：1 2 4-三唑衍生物 亲核取代 合成 结构表征 

分 类 号：R97[医药卫生—药品]