氨噻肟酸乙酯的合成研究  

The Synthesis of 2-(2-Aminothiazol-4-yl)-(Z)-2-(methoryimion)Acetate

作　　者：孙梦轲[1] 毕彩丰[1] 赵宇[1] 张震[1] 陈安成[1] 

机构地区：[1]中国海洋大学化学化工学院,海洋化学理论工程技术教育部重点实验室,山东青岛266100

出　　处：《精细化工中间体》2012年第2期27-29,59,共4页Fine Chemical Intermediates

摘　　要：以乙酰乙酸乙酯为原料,经肟化、甲基化、卤化及环合合成了(Z)-2-(2-氨基-4-噻唑)-2-甲氧基亚胺基乙酸乙酯。其中,肟化、甲基化无需分离提纯,简化了操作步骤,卤化过程用磺酰氯代替了传统的卤化试剂溴素,降低了反应的成本,并考察卤化反应中各因素对收率的影响。采用红外、核磁及液质连用色谱等确定其结构,通过高效液相色谱测定该工艺制得的氨噻肟酸乙酯的纯度可达到98%以上。产品的总收率达到46%(以乙酰乙酸乙酯计)。2-(2-Aminothiazol-4-yl)-(Z)-2-(methoryimion)acetate was synthesized from ethyl acetoacetate by oximation,methylation,halogenation and cyclic reaction in overall yield of 46%.The products from oximation and methylation were not necessary of separation and purification,therefore the process was simplified.Replacement of bromine with sulfuryl chloride as the halogenating reagent reduced the costs of the reaction.The influences of different factors on chlorination were investigated.The structure of the title compound was determined with FT-IR,1H NMR and LC-MS.

关 键 词：乙酰乙酸乙酯 氨噻肟酸乙酯 氯化 

分 类 号：TQ252.5[化学工程—有机化工]