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

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.