反应详情

Chloromethyl 2-thiopbenecarboxylate (0.63 g, 3.6 mmol) (Intermediate 6) in dry DMF (70 ml) is added dropwise at 50° C. to a solution of cesium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate (3.00 g, 3.9 mmol) and sodium iodide (28 mg, 0.19 mmol) in dry DMF (45 ml). The precipitate is removed by filtration after stirring for 4 hours and the solvent is removed at reduced pressure. The residue is dissolved in chloroform (50 ml) and washed four times with a saturated sodium hydrogen carbonate solution. After drying with magnesium sulfate the solvent is removed at reduced pressure to give the title compound:

1. customThe precipitate is removed by filtration
2. customthe solvent is removed at reduced pressure
3. dissolutionThe residue is dissolved in chloroform (50 ml)
4. washwashed four times with a saturated sodium hydrogen carbonate solution
5. dry with materialAfter drying with magnesium sulfate the solvent
6. customis removed at reduced pressure