造影剂碘海醇合成工艺的改进

Improved synthesis of iodinated contrast agent iohexol

以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、乙酸酐为起始原料,经酰化和水解合成中间体乙酰碘化物,再用缩水甘油烷基化反应生成碘海醇,采用异丙醇共沸带水进行重结晶,从而得到高纯度的碘海醇。合成产物经核磁共振(NMR)和质谱(MS)结构确证。结果表明,该工艺条件下反应总产率达65.52%,简单易操作,适合应用于工业化生产。

Iohexol is commonly used as iodinated contrast agent.A novel two-step synthesis process for iohexol is described.The process involves acylation and hydrolysis using 5-amino-N,N′-bis(2,3-dihydroxypropyl)-2,4,6-triiodol-1,3-phthalamide and acetic anhydride as starting materials to prepare acetyl iodide,followed by alkylating the acetyl iodide with glycidyl condensate to give crude iohexol.The crude iohexol can be purified by recrystallization which uses isopropanol and water to form an azeotrope.The overall yield was 65.52%and the structure of iohexol were confirmed by NMR and MS.This method is suitable for industrial production with easy operation.