反应详情

To a solution of 4-(4-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)-2-fluorophenoxy)picolinamide (2.5 g, 6.0 mmol) in EtOAc/MeCN/H2O (60 mL/60 mL/30 mL) was added iodobenzene diacetate (2.9 g, 9.0 mmol) at 0° C. The reaction was stirred at rt for 2 hours, then concentrated in vacuo. The resulted residue was dissolved with EtOAc (150 mL), washed with saturated aq. NaHCO3 (80 mL), dried over anhydrous Na2SO4, and concentrated in vacuo. The residue was washed with DCM/ether (1/10, 22 mL) to give the title compound as a yellow solid (2.09 g, 81% yield).

1. concentrationconcentrated in vacuo
2. dissolutionThe resulted residue was dissolved with EtOAc (150 mL)
3. washwashed with saturated aq. NaHCO3 (80 mL)
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. washThe residue was washed with DCM/ether (1/10, 22 mL)