反应详情

The 5-amino-2,4,6-triiodo-isophthaloyl dichloride (50 g, 84 mmol) was dissolved in anhydrous THF (200 ml), morpholine (29 ml, 333 mmol) was dissolved in 50 ml THF, and added dropwise to the solution over 1 hour. The mixture stirred overnight at ambient temperature. The crude product was loaded onto silica gel (100 g) and separated using a 750 g column eluting with DCM/EtOAc (1:1). This yielded 9 g of the [3-amino-2,4,6-triiodo-5-(morpholine-4-carbonyl)-phenyl]-morpholin-4-yl-methanone.

1. additionadded dropwise to the solution over 1 hour
2. customseparated
3. washeluting with DCM/EtOAc (1:1)