期刊信息
- 刊名： 河北师范大学学报（自然科学版）Journal of Hebei Normal University (Natural Science)
- 主办： 河北师范大学
- ISSN： 1000-5854
- CN： 13-1061/N
- 中国科技核心期刊
- 中国期刊方阵入选期刊
- 中国高校优秀科技期刊
- 华北优秀期刊
- 河北省优秀科技期刊
硫酸头孢喹肟中间体7-氨基头孢喹肟氢碘酸盐的合成
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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 -
DOI：10.13763/j.cnki.jhebnu.nse.2015.05.010
Synthesis of 7-amino Cefquinome Sulfate Hydroiodic Acid Salt as the Intermediate of Cefquinome Sulfate
摘要/Abstract
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 is 89.74% with these reaction conditions.7-amino cefquinome sulfate hydroiodic acid salt is characterized with elemental analysis and FT-IR.
关键词
参考文献 12
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