反应详情

温度

90 °C

5.0 gram 5-acetamino-N,N'-bis-(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzene-dicarboxamide (Compound 1), 0.36 gram of 25% sodium methoxide in methanol, and 1.5 gram glycidol are combined in 2-methoxyethanol and heated to 90° C. for four hours. Solvent is removed under vacuum followed by dissolution of the residue in water. The solution is treated with 1 gram each of Amberlyst A-15 and Amberlite IRA-67 ion-exchange resins to remove sodium methoxide. Water is removed under vacuum to afford an oil. Crystallization from methanol/isopropanol (10:75) afforded 3.5 gram (64.6%) iohexol.

1. customSolvent is removed under vacuum
2. dissolutionfollowed by dissolution of the residue in water
3. additionThe solution is treated with 1 gram each of Amberlyst A-15 and Amberlite IRA-67 ion-exchange resins
4. customto remove sodium methoxide
5. customWater is removed under vacuum
6. customto afford an oil
7. customCrystallization from methanol/isopropanol (10:75)