硫酸头孢喹肟中间体7氨基头孢喹肟氢碘酸盐的合成  

Synthesis of 7-amino Cefquinome Sulfate Hydroiodic Acid Salt as the Intermediate of Cefquinome Sulfate

作　　者：武晓青[1] 赵地顺[1,2] 尚青[1] 梁策 

机构地区：[1]河北科技大学化学与制药工程学院,河北石家庄050018 [2]河北省药物化工工程技术研究中心,河北石家庄050018 [3]河北新华科技兽药有限公司,河北石家庄050000

出　　处：《河北师范大学学报（自然科学版）》2015年第5期414-418,共5页Journal of Hebei Normal University：Natural Science

基　　金：国家自然科学基金(20976107)

摘　　要：7-氨基头孢喹肟(7-ACQ)氢碘酸盐是合成硫酸头孢喹肟的重要中间体.在氮气保护下,以7-氨基头孢烷酸(7-ACA)为原料,六甲基二硅胺烷为硅烷化试剂,对氨基、羧基保护后在三甲基碘硅烷的作用下与5,6,7,8-四氢喹啉反应生成7-ACQ氢碘酸盐.结果表明:基团保护、酯裂解、生成7-ACQ的反应时间分别为15,2,5h,反应温度分别为40,25,0℃,n(7-ACA)∶n(HMDS)∶n(TMSI)∶n(5,6,7,8-四氢喹啉)=1∶2.0∶1.4∶1.4,催化剂用量为0.2mL时,收率最高达89.74%.薄层色谱跟踪,并对目标产物进行了元素分析及红外光谱表征.The 7-amino cefquinome sulfate（7-ACQ）hydroiodic acid salt is a key intermediate in the preparation of cefquinome sulfate.7-amino cephalosporanic acid（7-ACA）was reacted with hexamethyldisilazane（HMDS）using trimethylsilyl iodide（TMSI）as catalyst to protect amino and carboxyl,further treated with trimethylsilyl iodide to obtain the iodization product,then the product was quaternized with 5,6,7,8-tetrahydroquinoline to give 7-ACQ hydroiodic acid salt.The three reactions were conducted in one pot under nitrogen atmosphere,monitored by TLC.The reaction times of the three steps are 15,2,5h,the temperatures are 40,25,0℃respectively.The mole ratio for n（7-ACA）∶n（HMDS）∶n（TMSI）∶n（5,6,7,8-tetrahydroquinoline）is 1∶2.0∶1.4∶1.4.The yield of 7-amino cefquinome sulfate hydroiodic acid salt is89.74% with these reaction conditions.7-amino cefquinome sulfate hydroiodic acid salt is characterized with elemental analysis and FT-IR.

关 键 词：硫酸头孢喹肟 7-氨基头孢烷酸 7-氨基头孢喹肟 合成 

分 类 号：O621.3[理学—有机化学]