碘克沙醇杂质的合成  

Synthesis of iodixanol impurities

作　　者：徐东强 王瑞华 王茴茴 高瑞阳 欧加保 程青芳 XU Dongqiang;WANG Ruihua;WANG Huihui;GAO Ruiyang;OU Jiabao;CHENG Qingfang(School of Pharmacy,Jiangsu Ocean University,Lianyungang 222005,China;Jiangsu Yutian Pharmaceutical Co.,Ltd.,Lianyungang 222000,China)

机构地区：[1]江苏海洋大学药学院,江苏连云港222005 [2]江苏宇田医药有限公司,江苏连云港222000

出　　处：《江苏海洋大学学报(自然科学版)》2025年第1期81-88,共8页Journal of Jiangsu Ocean University:Natural Science Edition

基　　金：连云港市科技成果转化“揭榜挂帅”专项资金资助项目(CA202101);江苏海洋大学研究生科研与实践创新计划项目(KYCX2023-53)。

摘　　要：为控制碘克沙醇质量,制备了碘克沙醇的5个杂质,分别为5-((3-(N-(3,5-双((2,3-二羟丙基)氨基甲酰基)-2,4,6-三碘苯基)乙酰氨基)-2-羟丙基)氨基)-N1,N3-双(2,3-二羟丙基)-2,4,6-三碘间苯二甲酰胺(杂质C)、N1,N3-双(2,3-二羟基丙基)-5-(N-(2-羟基-3-甲氧基丙基)乙酰氨基)-2,4,6-三碘间苯二甲酰胺(杂质D)、5-(N-(3-(N-(3-氨基甲酰基-5-((2,3-二羟丙基)氨基甲酰基)-2,4,6-三碘苯基)乙酰氨基)-2-羟丙基)乙酰氨基)-N1,N3-双(2,3-二羟丙基)-2,4,6-三碘间苯二甲酰胺(杂质E)、4-乙酰基-2-((N-(3,5-双((2,3-二羟丙基)氨基甲酰基)-2,4,6-三碘苯基)乙酰氨基)甲基)-N6,N8-双(2,3-二羟丙基)-5,7-二碘-3,4-二氢-2H-苯并[b][1,4]噁嗪-6,8-二甲酰胺(杂质G)、5-(N-(3-(N-(3,5-双((2,3-二羟丙基)氨基甲酰基)-2,4,6-三碘苯基)乙酰氨基)-2-羟丙基)乙酰氨基)-N1-(3-(2,3-二羟基丙氧基)-2-羟基丙基)-N3-(2,3-二羟基丙基)-2,4,6-三碘间苯二甲酰胺(杂质I),并通过MS和NMR对结构进行了确证。In order to control the quality of iodixanol,five impurities of iodixanol were prepared:5-(acetyl(3-((3,5-bis(((2,3-dihydroxypropyl)amino)carbonyl)-2,4,6-triiodophenyl)amino)-2-hydroxypropyl)amino)-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triodo-1,3-benzenedicarboxamide(impurity C),5-(acetyl(2-hydroxy-3-methoxypropyl)amino)-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triodo-1,3-Benzenedicarboxamide(impurity D),5-(acetyl(3-(acetyl(3-carbamoyl-5-((2,3-dihydroxypropyl)carbamoyl)-2,4,6-triodophenyl)amino)-2-hydroxypropyl)amino)-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triodobenzene-1,3-dicarboxamide(impurity E),4-acetyl-2-((acetyl(3,5-bis(((2,3-dihydroxypropyl)amino)carbonyl)-2,4,6-triodophenyl)amino)methyl)-N6,N8-bis(2,3-dihydroxypropyl)-3,4-dihydro-5,7-diodo-2H-1,4-Benzoxazine-6,8-dicarboxamide(impurity G),5-(acetyl-(3-(N-acetyl-3-((3-(2,3-dihydroxypropoxy)-2-hydroxypropyl)carbamoyl)-5-(2,3-dihydroxypropylcarbamoyl)-2,4,6-triiodoanilino)-2-hydroxypropyl)amino)-1-N,3-N-bis(2,3-dihydroxypropyl)-2,4,6-triodobenzene-1,3-dicarboxamide(impurity I),and the structures were confirmed by MS and NMR.

关 键 词：碘克沙醇 造影剂 杂质 合成 

分 类 号：TQ460.6[化学工程—制药化工]