合成头孢泊肟酯中间体的气相色谱跟踪分析

GC tracking analysis of synthesis of the intermediate of the cefpodoxime proxetil

目的 对合成头孢泊肟酯中间体 1-氯乙基氯甲酸酯、1-氯乙基异丙基碳酸酯 ,1-碘代乙基异丙基碳酸酯作定性、定量的跟踪分析 ,帮助确定最佳的合成工艺条件。方法 用 GC- MS、核磁共振、SE- 5 4(30 m×0 .5 3mm× 0 .2 5μm)毛细管柱气相色谱法进行定性、定量。结果 合成 1-氯乙基氯甲酸酯最高含量达 6 1.3%,1-氯乙基异丙基碳酸酯含量达 95 .4%,1-碘代乙基异丙基碳酸酯含量达 87.5 %。结论 实验表明本色谱方法分离度好 ,重现性好 ,对探索最佳合成工艺路线具有指导意义。

In this paper the quantitative and qualititative analyses for tracking of synthesis of 1-chloroethyl chloroformate,1-chloroethyl isopropyl carbonate and 1-iodoethyl isopropyl carbonate, the intermediates of the cefpodoxime proxetil, were described using GC-MS, 1 H -NMR and capillary column GC. Experiments showed that the method had good resolution and high reproducibility.