反应详情

To 217 g of diethylenetriamine (product commercially available) (2.1 mol), under stirring and under nitrogen atmosphere, 259 g of compound (A) 3-[(2-chloroacetyl) amino]-α-ethyl-2,4,6-triiodobenzenepropanoic acid (0.40 mol) are added. The mixture is kept at 50° C. for 3 h and, after cooling, is extracted with three 500-ml portions of CH2Cl2. After evaporation of the solvent, the residue is dissolved in 500 ml of H2O and acidified with 300 ml of 37% HCl. The resulting solution is counterflow extracted according to Craig with n-BuOH. A residue is obtained, which is purified as trihydrochloride by crystallisation in abs. EtOH after addition of 37% HCl. 187 g of 3-[[[2-[(2-aminoethyl)amino]ethyl]amino]acetylamino]-α-ethyl-2,4,6-triiodobenzenepropanoic acid (0.227 mol) are obtained.

1. temperatureafter cooling
2. extractionis extracted with three 500-ml portions of CH2Cl2
3. customAfter evaporation of the solvent
4. dissolutionthe residue is dissolved in 500 ml of H2O
5. extractionextracted
6. customA residue is obtained
7. customwhich is purified as trihydrochloride by crystallisation in abs
8. additionEtOH after addition of 37% HCl