反应详情

5-Acetoxyacetamido-N,N'-bis[(2,3-dihydroxypropyl)-2-hydroxyethyl]-2,4,6-triiodoisophthalamide (77 g, 0.086 g-mole) is dissolved in 270 ml of hot water containing 8.2 g (0.08 g-mole) sulfuric acid. The solution is stirred and heated at 95°-100° C. to hydrolyze the acetate. At the end of the reaction, the solution is cooled to room temperature and deionized using an anionic exchange resin, IRA-93 (Rohm and Haas Co.) to remove sulfuric acid. The solution is then concentrated and the crude product is purified by preparative liquid chromatography to provide the purified desired product (51 g; 0.06 g-mole, 70% yield). The 13C nmr spectra are consistent with the structure. The HPLC purity is 99.1% (C18, H2O/MeOH; 95/5). The water solubility (w/v) is 100%; the iv LD50 in mice is 5 g I/kg (based on iodine content). Osmolality: 676 mOsm/kg (32% I); viscosity: 8.2 cps (37°), 10.0 cps (25 °) (32% I).

1. temperatureheated at 95°-100° C.
2. customAt the end of the reaction
3. customto remove sulfuric acid
4. concentrationThe solution is then concentrated
5. customthe crude product is purified by preparative liquid chromatography
6. customto provide the