碘海醇、碘克沙醇中间体水解物的合成工艺改进  

Improvement of Synthesis Process of Hydrolysate of Iodohydol and Iodoxanol Intermediates

作　　者：段香江 陈曦 林照棋 任方振 Duan Xiangjiang;Chen Xi;Lin Zhaoqi;Ren Fangzhen(Zhejiang Haizhou Pharmaceutical Co.,Ltd.,Zhejiang,318000)

机构地区：[1]浙江海洲制药股份有限公司,浙江318000

出　　处：《当代化工研究》2024年第17期176-178,共3页Modern Chemical Research

摘　　要：研究碘海醇、碘克沙醇中间体水解物的合成工艺改进实验内容,以提升物质合成质量。通过对照原有工艺水合物合成发现,5-氨基-N,N'-双(2,3-二羟基丙基)-2,4,6-三碘-1,3-苯二甲酰胺乙腈占比为35%、水为65%;5-乙酰氨基-N,N'-二(2,3二羟基丙基)-1,3-苯二甲酰胺流动相A为水;流动相B中,获取梯度洗脱时间为0 min至1 h,水含量百分率为99%~87%,乙腈为1%~13%;总收率,89.8%;mp,274~277℃。整体合成效果在时间、成本、生产方面均有提升,因此可在后续长期使用。The synthetic process of the intermediate hydrolysate of iohexol and iodixanol was studied,and the experimental contents were improved to improve the synthetic quality of substances.Compared with the original process of hydrate synthesis,it is found that 5-amino-n;The ra-tio of N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzamide acetonitrile is 35%and water is 65%;The mobile phase a of 5-acetamido-n,n'-bis(2,3 dihydroxypropyl)-1,3-benzamide is water;In mobile phase B,the gradient elution time is 0min to 1h,the percentage of water content is 99%~87%,and acetonitrile is 1%~13%;The total yield was 89.8%;mp,274~277℃.The overall synthesis effect has been improved in terms of time,cost and production,so it can be used for a long time in the future.

关 键 词：碘海醇 碘克沙醇 水解物 合成工艺 5-氨基-N N'-双(2 3-二羟基丙基)-2 4 6-三碘-1 3-苯二甲酰胺 5-乙酰氨基-N N'-二(2 3二羟基丙基)-1 3-苯二甲酰胺 

分 类 号：TQ460.6[化学工程—制药化工]