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 (4 mmol) in 1,4-dioxane (20 mL) was added ˜11 equivalents of 20% phosgene solution in toluene (44 mL) at ambient temperature. The flask was sealed and the solution was heated at 60° C. for 15 hours. The reaction was allowed to cool to ambient temperature and then concentrated at reduced pressure to yield an off white, semi-crystalline solid. Dioxane (50 mL×2) was added and removed slowly at reduced pressure to give an off white, semi-crystalline solid. The material was used without further purification.

1. customThe flask was sealed
2. temperatureto cool to ambient temperature
3. concentrationconcentrated at reduced pressure
4. customto yield an off white, semi-crystalline solid
5. customremoved slowly at reduced pressure
6. customto give an off white, semi-crystalline solid
7. customThe material was used without further purification