反应详情

To a solution of N,N'-Bis[2-(acetyloxy)-1-[(acetyloxy)methyl]ethyl]-2,4,6-triiodo-5-[3-(iodomethyl)-5-oxo-4-morpholinyl]-1,3-benzenedicarboxamide of example 7b (2.01 g, 1.83 mmol) in glacial acetic acid (35 ml), was added silver acetate (0.67 g, 4 mmol) and the mixture refluxed for 14 hours. The solvent was removed in vacuo at 40°, and the residue extracted with ethyl acetate (200 ml). The organic extract, after washing with saturated aqueous sodium bicarbonate (3×25 ml) and water (3×25 ml), was dried over anhydrous sodium sulfate. Removal of the solvent followed by purification of the crude product by column chromatography over silica gel, yielded analytically pure N,N'-Bis[2-(acetyloxy)-1-[(acetyloxy)methyl]ethyl]-5-[3[(acetyloxy)methyl]-5-oxo-4-morpholinyl]-2,4,6-triiodo-1,3-benzenedicarboxamide as a white fluffy solid (1.5 g, 82% yield), m.p. 208°-210°.

1. temperaturethe mixture refluxed for 14 hours
2. customThe solvent was removed in vacuo at 40°
3. extractionthe residue extracted with ethyl acetate (200 ml)
4. washThe organic extract, after washing with saturated aqueous sodium bicarbonate (3×25 ml) and water (3×25 ml)
5. dry with materialwas dried over anhydrous sodium sulfate
6. customRemoval of the solvent
7. customfollowed by purification of the crude product by column chromatography over silica gel