反应详情

3-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline (1.32 g, 2.1 mmol) was dissolved in pyridine (10 ml) containing acetic anhydride (10 ml). The mixture was stirred at room temperature for 2 h and CH2Cl2 (100 ml) and the solution was washed with water (3×25 ml). The organic phase was washed with water (3×50 ml) and a saturated aqueous solution of NaHCO3 (2×50 ml). After drying (Na2SO4) and evaporation, the residue was purified by flash chromatography on a silica column using a mixture of CH2Cl2 and methanol (95:5) as the eluent. Yield: 1.30 g (82%).

1. washCH2Cl2 (100 ml) and the solution was washed with water (3×25 ml)
2. washThe organic phase was washed with water (3×50 ml)
3. customAfter drying
4. custom(Na2SO4) and evaporation
5. customthe residue was purified by flash chromatography on a silica column
6. additiona mixture of CH2Cl2 and methanol (95:5) as the eluent