反应详情

Chloromethyl 4-methoxy-3-methylbenzoate (Intermediate 8) (2.38 g, 11.0 mmol) in dry DMF (100 ml) is added dropwise at 50° C. to a solution of potassium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate (6.7 0 g, 10.0 mmol) and sodium iodide (75 mg, 0.50 mmol) in dry DMF (140 ml). The precipitate is removed by filtration after stirring for 4.5 hours and 16 hours at room temperature, and the solvent is removed at reduced pressure. The residue is dissolved in chloroform (100 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 (100 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