反应详情

5-Acetoxyacetamido-N,N'-bis[(2,3-dihydroxypropyl)-2-hydroxyethyl]-2,4,6-triiodoisophthalamide. 69 g (0.1 g-mole) of 5-acetoxyacetamido-2,4,6-triiodoisophthaloyl chloride is dissolved in DMAc (140 ml) and anhydrous Na2CO3 (31.8 g, 0.3 g-mole) is added. To the solution, a DMAc solution (87 ml) containing 26.2 g (0.3 g-mole) of 3-(N-2-hydroxyethyl)amino-1,2-propanediol is added. The mixture is heated and stirred at 35°-40° C. until the reaction is completed as determined by the TLC analysis (EtOAc/CH2Cl2 ; 30/20). After the reaction, the inorganic salts are filtered and the filtrate containing the desired product is evaporated to dryness to give a gum. The gum is triturated with isopropyl alcohol to dissolve the excess amino-triol. The clear supernatant is decanted and the residual solid is dissolved in water (150 ml), treated with Amberlite® IR-120H resin and evaporated to dryness to give the desired product (77 g, 86% yield).

1. additionis added
2. temperatureThe mixture is heated
3. customAfter the reaction
4. filtrationthe inorganic salts are filtered
5. additionthe filtrate containing the desired product
6. customis evaporated to dryness
7. customto give a gum
8. customThe gum is triturated with isopropyl alcohol
9. dissolutionto dissolve the excess amino-triol
10. customThe clear supernatant is decanted
11. dissolutionthe residual solid is dissolved in water (150 ml)
12. additiontreated with Amberlite® IR-120H resin
13. customevaporated to dryness