反应详情

5-Amino-3-acetoxymethyl-2,4,6-triiodobenzoic acid (43.9 g, 0.075 mol) was suspended in 1,2-dichloroethane (40 ml) and thionyl chloride (24.9 ml, 0.34 mol) was added. The mixture was heated to reflux temperature for 3 h. After evaporation to dryness, the residue was dissolved in tetrahydrofuran (50 ml). Sodium hydrogen carbonate (15 g) and crystalline sodium carbonate (5 g) were added to the solution and the mixture was stirred at room temperature for 3 h. The mixture was filtered and the filtrate evaporated to dryness. After pump-drying, a foam was formed, yield 44.6 g (98%). This material was used directly in the next step.

1. temperatureThe mixture was heated
2. temperatureto reflux temperature for 3 h
3. customAfter evaporation to dryness
4. dissolutionthe residue was dissolved in tetrahydrofuran (50 ml)
5. additionSodium hydrogen carbonate (15 g) and crystalline sodium carbonate (5 g) were added to the solution
6. filtrationThe mixture was filtered
7. customthe filtrate evaporated to dryness
8. customAfter pump-drying
9. customa foam was formed