反应详情

温度

50 °C

1-Chloroethyl ethyl carbonate (10.00 g, 66.0 mmol) was added dropwise during 1.5 hour at room temperature to a solution of potassium 5-(N-acetylamino)3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate (40.00 g, 60.0 mmol) and sodium iodide (0.89 g, 6.0 mmol) in dry dimethylformamide (200 ml). After stirring at 50° C. for 24 hours the solvent was removed at reduced pressure. The residue was dissolved in chloroform (120 ml) and washed four times with a saturated sodium hydrogen carbonate solution and twice with water. After drying with magnesium sulfate, treatment with activated charcoal and filtration, the title compound was crystallised by concentrating the solution at reduced pressure. Yield: (79%). Purity by HPLC: 99%. 1H-NMR (DMSO-d6): delta=1.25 (t, J=7 Hz, CH3); 1.64 (d, J=6 Hz, CH3); 1.67 (s, N(Me)COCH3); 2.05(s, NCOCH3); 2.96 (s, NCH3); 4.21 (q, J=7 Hz, CH2); 6.97 (q, J=6 Hz, CH); 10.10 ppm (s, NH).

1. customwas removed at reduced pressure
2. dissolutionThe residue was dissolved in chloroform (120 ml)
3. washwashed four times with a saturated sodium hydrogen carbonate solution
4. dry with materialAfter drying with magnesium sulfate, treatment with activated charcoal and filtration
5. customthe title compound was crystallised
6. concentrationby concentrating the solution at reduced pressure