反应详情

5-Amino-2,4,6-triiodo-N,N'-bis(2,3-dihydroxypropyl)-isophthalamide (14.08 g, 0.02 mol), which had been prepared according to GB-A-1548594 was suspended in pyridine (200 ml) and acetic anhydride (57.1 g, 0.56 mol) was added dropwise with stirring and cooling. After stirring overnight, the mixture was poured into ethyl acetate (300 ml) and 20% aqueous HCl (200 ml). After extraction, the organic phase was washed with 2 M aqueous HCl (20 ml), brine (70 ml), dried (Na2SO4) and evaporated. Yield 17.4 g (100%). The crude material was used without further purification, since analysis by HPLC and 1H NMR indicated, that the product was >97% pure.

1. temperaturecooling
2. stirringAfter stirring overnight
3. extractionAfter extraction
4. washthe organic phase was washed with 2 M aqueous HCl (20 ml), brine (70 ml)
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customThe crude material was used without further purification, since analysis by HPLC and 1H NMR