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p H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。
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.
作者
赵民军
赵燕青
厉昆
厉梦琳
彭荣花
郭俊杰
ZHAO Min-jun;ZHAO Yan-qing;LI Kun;LI Meng-lin;PENG Rong-hua;GUO Jun-jie(Apeloa Pharmaceutical Co.,Ltd.,Dongyang 322118,China;Zhejiang Apeloatospo Pharmaceutical Co.,Ltd.,Dongyang 322118,China)
出处
《精细化工中间体》
CAS
2024年第4期34-38,41,共6页
Fine Chemical Intermediates
