![PROCESS FOR THE PREPARATION OF IOPAMIDOL](/ep/2018/04/18/EP3066071B1/abs.jpg.150x150.jpg)
基本信息:
- 专利标题: PROCESS FOR THE PREPARATION OF IOPAMIDOL
- 专利标题(中):制备IOPAMIDOL的方法
- 申请号:EP14796024.9 申请日:2014-11-04
- 公开(公告)号:EP3066071B1 公开(公告)日:2018-04-18
- 发明人: BATTISTINI, Elisa , BUONSANTI, Federica , IMPERIO, Daniela , LATTUADA, Luciano , NAPOLITANO, Roberta
- 申请人: Bracco Imaging S.p.A.
- 申请人地址: Via E. Folli 50 20134 Milano IT
- 专利权人: Bracco Imaging S.p.A.
- 当前专利权人: Bracco Imaging S.p.A.
- 当前专利权人地址: Via E. Folli 50 20134 Milano IT
- 代理机构: Ravizza, Claudio
- 优先权: EP13191551 20131105
- 国际公布: WO2015067601 20150514
- 主分类号: C07C231/02
- IPC分类号: C07C231/02 ; C07F5/02 ; C07F5/04
摘要:
The present invention discloses a process for the preparation of Iopamidol of formula (II) and comprising the following steps: a) reacting the Compound (I) wherein X is OR2 or R3, and wherein R2 and R3 are a Ci-C6 linear or branched alkyl, C3-C6 cycloalkyl, C6 aryl, optionally substituted with a group selected from the group consisting of methyl, ethyl, n-propyl, i-propyl, n-butyl, sec-butyl, t-butyl and phenyl, with the acylating agent (S)-2-(acetyloxy)propanoyl chloride in a reaction medium to provide the acetyloxy derivative of Compound (I); b) hydrolyzing the intermediate from step a) with an aqueous solution at a pH comprised from 0 to 7, by adding water or a diluted alkaline solution such as sodium hydroxide or potassium hydroxide, freeing the hydroxyls from the boron-containing protective groups, obtaining the N—(S)-2-(acetyloxy)propanoyl derivative of Compound (II); c) alkaline hydrolysis to restore the (S)-2-(hydroxy)propanoyl group and to obtain Iopamidol (II) and optional recovery of the boron derivative from the solution obtained in step b). The boron-containing protective group is versatile, efficient and recyclable. A one-pot synthesis, without intermediate isolation is provided, leading to a decreasing of recovered and recycled solvents and a significant increasing in the yield, representing a significant advantage in terms of cost-effectiveness of the entire process and environmental awareness.
公开/授权文献:
- EP3066071A1 PROCESS FOR THE PREPARATION OF IOPAMIDOL 公开/授权日:2016-09-14
IPC结构图谱:
C | 化学;冶金 |
--C07 | 有机化学 |
----C07C | 无环或碳环化合物 |
------C07C231/00 | 羧酸酰胺的制备 |
--------C07C231/02 | .通过与氨或胺反应从羧酸或从它们的酯、酐或卤化物来制备 |