摘要
3′-碘甲基头孢噻肟是合成硫酸头孢喹肟的重要中间体.其中间体3′-碘甲基头孢噻肟是以头孢噻肟为原料与三甲基碘硅烷反应生成.在氮气保护下,选用无水二氯甲烷为溶剂所得产物效果最佳.最佳工艺条件是:三甲基碘硅烷与头孢噻肟物质的量比为1.4∶1,反应温度30℃,反应时间2h,硫酸头孢喹肟中间体(碘代物)的收率为96.6%.最后,对产品结构进行了核磁共振波谱、红外光谱表征.
The 3＇-iodomethyl cephalosporins are useful intermediates in the preparation of sulfate. Intermediate of cefquinome sulfate 3′-iodomethyl cephem was synthesized by reacting cefquinome cefotaxime and trimethylsilyl iodide. The reaction condition is to use dry dichloromethane as solvent and under the dry nitrogen protected. Optional conditions for the synthesis of 3′-iodomethyl cephem were obtained, trimethylsilyl iodide and cefotaxime molar ratio of 1.4 ： 1, reaction temperature 30 ℃ and reaction time 2 h. Under the optimal conditions, the yield of intermediate of cefquinome sulfate-iodide was up to 96.6 %^. Finally,the structures of products were characterized by means of ^1HNMR and IR.
出处
《河北师范大学学报（自然科学版）》
CAS
北大核心
2013年第6期595-598,共4页
Journal of Hebei Normal University：Natural Science
基金
国家自然科学基金(20976107)
