反应详情

温度

50 °C

1-Chloroethyl thenyl carbonate (2.43 g, 11 mmol) was added at room temperature to a solution of potassium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate (6.66 g, 10 mmol) and potassium iodide (0.17 g, 1 mmol) in dry DMF. After stirring at 50° C. for 5 hours and at room temperature for 4 days the solvent was removed at reduced pressure. The residue was suspended in chloroform (100 ml) and washed three times with a saturated sodium hydrogen carbonate solution and finally twice with water. After drying with magnesium sulfate the solution was evaporated to dryness. Yield: 7.9 g. Purity by HPLC: 88%. 1H-NMR (DMSO-d6): delta=1.64 (CHCH3); 1.65 (N(CH3)COCH3); 2.05 (NCOCH3 ); 2.95 (NCH3); 5.41 (CH2); 7.00 (CHCH3); 7.05; 7.25; 7.61 (thiophene); 10.11 ppm (NH).

1. customwas removed at reduced pressure
2. washwashed three times with a saturated sodium hydrogen carbonate solution
3. dry with materialAfter drying with magnesium sulfate the solution
4. customwas evaporated to dryness