以草酸二甲酯为原料高效合成2,2’-双(2-噁唑啉)  

Efficient synthesis of 2,2’-bis(2-oxazoline)from dimethyl oxalate

作　　者：葛浩栋 吴林波[1,2] GE Haodong;WU Linbo(State Key Laboratory of Chemical Engineering,College of Chemical and Biological Engineering,Zhejiang University,Hangzhou 310058,China;Key Laboratory of Biomass Chemical Engineering of Ministry of Education,College of Chemical and Biological Engineering,Zhejiang University,Hangzhou 310058,China)

机构地区：[1]浙江大学化学工程联合国家重点实验室,化学工程与生物工程学院,杭州310058 [2]浙江大学生物质化工教育部重点实验室,化学工程与生物工程学院,杭州310058

出　　处：《化学工业与工程》2025年第1期9-18,共10页Chemical Industry and Engineering

摘　　要：针对2,2’-双(2-噁唑啉)(BOZ)合成存在原料成本高、反应时间长、产率低和提纯复杂等问题,以草酸二甲酯(DMO)和乙醇胺(MEA)为原料,采用三步法合成BOZ,最适宜条件为:在乙醇中,n(MEA)∶n(DMO)按2.6∶1.0在40℃反应20 min得到N,N-双(2-羟乙基)乙二酰胺(BHEOA);在甲苯中,n(BHEOA)∶n(SOCl_(2))按1∶3在50~90℃逐步升温反应得到N,N-双(氯乙基)乙二酰胺(BCEOA);最后在含吸水剂的乙醇中,n(BCEOA)∶n(NaOH)按1∶2回流反应1 h得到BOZ。3步产率分别为98.1%、96.3%和73.6%。第3步所得滤液经二次结晶,产率进一步提高到85.8%。In view of the problems in the synthesis of 2,2’-bis(2-oxazoline)(BOZ),such as high cost of raw materials,long reaction time,low yield and complex purification,BOZ was synthesized from dimethyl oxalate(DMO)and ethanolamine(MEA)via a three-step method.The optimum conditions were as follows:First,in ethanol,DMO and MEA reacted at molar ratio of 1∶2.6 at 40℃for 20 min to obtain N,N-bis(2-hydroxyethyl)acetamide(BHEOA).Then in toluene,BHEOA and SOCl_(2) reacted at molar ratio of 1∶3 at 50 to 90℃to obtain N,N-bis(chloroethyl)acetamide(BCEOA).Finally,in ethanol containing water absorbent,BCEOA and NaOH reacted at molar ratio of 1∶2 at reflux temperature for 1 h to obtain BOZ.The yields of the three steps were 98.1%,96.3%and 73.6%respectively.After secondary crystallization of the filtrate in the third step,the yield increased to 85.8%.

关 键 词：扩链剂 2 2’-双(2-噁唑啉) 草酸二甲酯 

分 类 号：O629[理学—有机化学]