一种头孢母核氢碘酸盐一水晶型化合物的合成
Synthesis of a Crystal Compound of Cephalosporin Nucleate Hydroiodate
赵民军 1赵燕青 2厉昆 1厉梦琳 2彭荣花 2郭俊杰2
作者信息
- 1. 普洛药业股份公司,浙江 东阳 322118
- 2. 浙江普洛得邦制药有限公司,浙江 东阳 322118
- 折叠
摘要
在溶剂中六甲基二硅烷与碘反应制备成三甲基碘硅烷;7-氨基头孢烷酸(7-ACA)与六甲基二硅氮烷(HMDS)在咪唑氢碘酸盐催化下进行硅烷化保护后,加入三甲基氯硅烷、N,N-二乙基苯胺;加入三甲基碘硅烷进行卤化反应,加入吡啶进行取代反应,加入溶剂和水淬灭,得到7-氨基-3-(1-吡啶甲基)头孢烯酸碘化盐和氯化氢混合物;混合物通过加酸溶解、脱色,加入碘化钾,碱液调节pH析晶;得到类白色7-氨基-3-(1-吡啶甲基)头孢烯氢碘酸盐一水晶型化合物.化合物纯度99.28％(HPLC),PXRD检测具有晶型特性,加速稳定性良好.
Abstract
Prepare trimethyliodosilane by reacting hexamethyldisilane with iodine in a solvent.After silanization protection of 7-aminocephalosporin acid(7-ACA)and hexamethyldisilazane(HMDS)catalyzed by imidazolium hydroiodide,trimethylchlorosilane and N,N-diethylaniline were added.Add trimethyliodosilane for the halogenation reaction,then add pyridine for substitution reaction,add solvent and use water quenching to obtain a mixture of 7-amino-3-(1-pyridylmethyl)cephalosporin acid iodide and hydrogen chloride;The mixture is dissolved and faded by adding acid,potassium iodide is then added,and the pH is adjusted by alkaline solution for crystallization;This process obtains a crystal like compound of white 7-amino-3-(1-pyridylmethyl)cephalosporin hydroiodate.The compound purity is of 99.28％(HPLC),PXRD detection has crystalline characteristics and good acceleration stability.
关键词
7-ACA/晶型/三甲基碘硅烷Key words
7-ACA/crystal type/trimethyliodosilane引用本文复制引用
出版年
2024
NETL
NSTL
维普
万方数据