反应详情

温度

60 °C

To a solution of acetic acid 1-acetoxymethyl-2-[3-amino-5-(2,3-diacetoxy-propylcarbamoyl)-2,4,6-triiodo-benzoylamino]-ethyl ester (15 g, 17 mmol) in 1,4-dioxane (40 mL) was added a solution of 20% phosgene in toluene (100 mL, 11 eq) at ambient temperature. The mixture was then heated to 60° C. for 15 hours. The reaction mixture was cooled to ambient temperature and then concentrated at reduced pressure to give an off white solid. Dioxane (50 mL×2) was added and removed slowly at reduced pressure to give an off-white solid which was placed on a vacuum line to remove any residual solvent. The material was used without further purification

1. temperatureThe reaction mixture was cooled to ambient temperature
2. concentrationconcentrated at reduced pressure
3. customto give an off white solid
4. customremoved slowly at reduced pressure
5. customto give an off-white solid which
6. customto remove any residual solvent
7. customThe material was used without further purification