反应详情

Add benzyl chloroformate (5.96 mL, 41.77 mmol) to a solution of 5-iodo-N-methyl-N-propyl-isophthalamic acid (14.5 g, 41.77 mmol), triethylamine (6.4 mL, 45.95 mmol) and 4-dimethylaminopyridine (2.55 g, 20.88 mmol) in dichloromethane (125 mL) at 0° C. and at room temperature for 40 h. Wash the solution twice with a saturated aqueous solution of NaHCO3, 5% aqueous solution of potassium hydrogen sulfate, saturated aqueous sodium chloride, dry (magnesium sulfate), and concentrate. Dissolve the crude in dichloromethane, wash with a 0.5 N NaOH solution, H2O, saturated aqueous sodium chloride, dry (magnesium sulfate) and concentrate to give the title compound (6 g, 33%).

1. washWash the solution twice with a saturated aqueous solution of NaHCO3, 5% aqueous solution of potassium hydrogen sulfate, saturated aqueous sodium chloride
2. dry with materialdry (magnesium sulfate)
3. concentrationconcentrate
4. dissolutionDissolve the crude in dichloromethane
5. washwash with a 0.5 N NaOH solution, H2O, saturated aqueous sodium chloride
6. dry with materialdry (magnesium sulfate)
7. concentrationconcentrate