反应详情

温度

50 °C

To a solution of [3-Amino-2,4,6-triiodo-5-(morpholine-4-carbonyl)-phenyl]-morpholin-4-yl-methanone (8 g, 11.4 mmol) in 1,4-dioxane (40 mL) was added ˜11 equivalents of 20% phosgene solution in toluene (60 mL, 120 mmol) at ambient temperature, the solution was heated at 50° 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 (30 mL×2) was added and removed slowly at reduced pressure to give a light brown, semi-crystalline solid which was placed on a vacuum line to remove any residual solvent. The material was used without further purification.

1. temperatureto cool to ambient temperature
2. concentrationconcentrated at reduced pressure
3. customto yield an off white, semi-crystalline solid
4. customremoved slowly at reduced pressure
5. customto give a light brown, semi-crystalline solid which
6. customto remove any residual solvent
7. customThe material was used without further purification