Reaktion #65062

Reaktionsgleichung

4-Chloro-1,3-dioxolan-2-one

potassium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate

sodium iodide

→

1,3-Dioxolan-2-one-4-yl-5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas removed at reduced pressure
2. 2
   workup.DISSOLUTIONThe residue was dissolved in chloroform (100 ml)
3. 3
   Waschenwashed four times with a saturated sodium hydrogen carbonate solution
4. 4
   SonstigeAfter treatment with magnesium sulfate the solution was finally evaporated to dryness

Vorschrift

4-Chloro-1,3-dioxolan-2-one (1.35 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 sodium iodide (0.15 g, 1 mmol) in dry DMF (50 ml). After stirring at 50° C. for 6 hours and at room temperature for 4 days the solvent was removed at reduced pressure. The residue was dissolved in chloroform (100 ml) and washed four times with a saturated sodium hydrogen carbonate solution and finally twice with water. After treatment with magnesium sulfate the solution was finally evaporated to dryness. Yield: 5.6 g. Purity by HPLC: 93%. 1H-NMR (DMSO-d6): delta=1.67 (N(CH3)COCH3); 2.05(NCOCH3); 2.96(NCH3); 4.7; 4.9(CH2); 7.02(CH); 10.14 ppm(NH).

Quelle