反应详情

5-Amino-3-acetoxymethyl-N-(2,3-diacetoxypropyl)-2,4,6-triiodobenzamide (3.0 g, 4.03 mmol) was dissolved in dry N,N-dimethylacetamide (8 ml) at ambient temperature. With efficient stirring acetoxyacetyl chloride (4.39 ml, 40.3 mmol) was added dropwise, and the mixture was stirred overnight. The mixture was then added slowly with stirring into a saturated solution of sodium hydrogen carbonate (80 ml). The precipitate formed was filtered off and dissolved in chloroform (80 ml). The organic solution was washed with an aqueous saturated solution of NaHCO3 (25 ml), and then evaporated to dryness. The solid residue was dissolved in acetone and filtered through a pad of alumina with acetone as eluent. Evaporation of the solvent gave 3.38 g (100%) of a white crystalline product.

1. additionwas added dropwise
2. additionThe mixture was then added slowly
3. customThe precipitate formed
4. filtrationwas filtered off
5. dissolutiondissolved in chloroform (80 ml)
6. washThe organic solution was washed with an aqueous saturated solution of NaHCO3 (25 ml)
7. customevaporated to dryness
8. dissolutionThe solid residue was dissolved in acetone
9. filtrationfiltered through a pad of alumina with acetone as eluent
10. customEvaporation of the solvent