反应详情

温度

60 °C

3-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline (3.3 g, 5.3 mmol) was suspended in glacial acetic acid (12 ml) containing acetic anhydride (48 ml) and concentrated sulfuric acid (0.08 ml). The mixture was stirred at 60° C. for 3 h, allowed to cool to room temperature, and CH2Cl2 (100 ml) and water (100 ml) were added. The organic phase was washed with water (3×50 ml) and a saturated aqueous solution of NaHCO3 (2×50 ml). After drying (MgSO4) and evaporation, the residue was dissolved in a mixture of CH2Cl2 and methanol (9:1) and filtered through a short silica pad and evaporated. Yield: 3.0 g (71%).

1. temperatureto cool to room temperature
2. washThe organic phase was washed with water (3×50 ml)
3. customAfter drying
4. custom(MgSO4) and evaporation
5. dissolutionthe residue was dissolved in a mixture of CH2Cl2 and methanol (9:1)
6. filtrationfiltered through a short silica pad
7. customevaporated