反应详情

2,3,5-triiodobenzoic acid (25 g), 2-hydroxyethyl methacrylate (7.2 g), 1,3-dicyclohexylcarbodiimide (11.5 g) and 4-pyrrilidinopyridine (0.75 g) were stirred in ether suspension (250 ml) at room temperature for 24 hr. The solid was filtered off and the residue washed with fresh ether. The ether solution was extracted with dilute HCl (0.2M) and then with saturated sodium bicarbonate solution. The organic phase was dried (MgSO4) and the solvent removed under reduced pressure. The residue (21.1 g) was recrystallised from ethyl acetate to give a pure material as white crystals m.pt.94° C.

1. filtrationThe solid was filtered off
2. washthe residue washed with fresh ether
3. extractionThe ether solution was extracted with dilute HCl (0.2M)
4. dry with materialThe organic phase was dried (MgSO4)
5. customthe solvent removed under reduced pressure
6. customThe residue (21.1 g) was recrystallised from ethyl acetate