口服抗生素头孢克肟杂质EP-E的合成及其结构确证  

Synthesis and Structure Confirmation of Impurity EP-E in Oral Antibiotic Cefixime

作　　者：陶志远 厉昆 阳学文 陈亮 杨硕 周若楠 李啸风[3] TAO Zhi-yuan;LI Kun;YANG Xue-wen;CHEN Liang;YANG Shuo;ZHOU Ruo-nan;LI Xiao-feng(Zhejiang Apeloatospo Pharmaceutical Co.,Ltd.,Dongyang 322118,China;Apeloa Pharmaceutical Co.,Ltd.,,Dongyang 322118,China;Department of Chemistry,Zhejiang University,Hangzhou 310027,China)

机构地区：[1]浙江普洛得邦制药有限公司,浙江东阳322118 [2]普洛药业股份公司,浙江东阳322118 [3]浙江大学化学系,浙江杭州310027

出　　处：《精细化工中间体》2023年第2期44-46,63,共4页Fine Chemical Intermediates

摘　　要：以(6R,7R)-7-氨基-8-氧代-3-甲基-5-硫杂-1-氮杂双环[4.2.0]辛-2-烯-2-羧酸(7-ADCA)与(Z)-2-(2-氨基噻唑-4-基)-2-乙酰氧亚氨基硫代乙酸(S-2-苯并噻唑)酯为起始原料进行酰化反应、碳酸钾水解、硫酸酸化得到头孢克肟杂质EP-E,纯度98.2%(HPLC),收率95.8%,其结构经LS-MS、^(1)H NMR、^(13)C NMR和IR表征确证。Using(6R,7R)-7-amino-8-oxo-3-methyl-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid(7-ADCA) and(Z)-2-(2-aminothiazol-4-yl)-2-acetoxyiminothioacetic acid(S-2-benzothiazole) ester as starting materials,EP-E was obtained by hydrolysis with potassium carbonate and acidification with sulfuric acid with HPLC was 98.2% and yield was 95.8%.The structure of the obtained compound was confirmed by LSMS,1H NMR,13C NMR and IR.

关 键 词：杂质 活性酯 7-ADCA 

分 类 号：R97[医药卫生—药品]