反应详情

温度

50 °C

1-Chloroethyl octadecyl carbonate (7.54 g, 20 mmol) was added at room temperature to a solution of potassium 5-acetamido-3-(N-methylacetamido)-2,4,6-triiodobenzenecarboxylate (15.99 g, 24 mmol) and potassium iodide (0.33 g, 2 mmol) in dry N,N-dimethylformamide. After stirring at 50° C. for 18 hours the solvent was removed at reduced pressure. The residue was suspended in chloroform (200 ml) and washed three times with a saturated sodium bicarbonate solution and finally twice with water. After drying with magnesium sulphate the solvent was removed at reduced pressure. Yield: 18.6 g. The product was further purified by flash chromatography (Silicagel 60, chloroform/acetonitrile 85:15). 1H NMR (DMSO-d6): δ 0.852(CH2CH3), 1.236(CH2), 1.639(CHCH3),1.657(COOCH2CH2), 1.670(N(CH3)COCH3), 2.051(NCOCH3),2.965(NCH3), 4.154(COOCH2), 6.971 (CHCH3),10.103 (NH).

1. customwas removed at reduced pressure
2. washwashed three times with a saturated sodium bicarbonate solution
3. dry with materialAfter drying with magnesium sulphate the solvent
4. customwas removed at reduced pressure
5. customThe product was further purified by flash chromatography (Silicagel 60, chloroform/acetonitrile 85:15)