HRID870417

反应详情

EQUATION

反应方程式

HRID 870417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of 3-chloro-4-(4-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)-2-fluorophenoxy)picolinamide (437 mg, 0.88 mmol) in EtOAc (5 mL), CH3CN (5 mL) and H2O (2.5 mL) was added iodobenzene diacetate (341 mg, 1.06 mmol) at 0° C. The reaction was stirred at 0° C. for 30 minutes, then warmed up to rt and continued to stir for 3 hours. The mixture was concentrated in vacuo, and the residue was purified by a silica gel column chromatography (PE/EtOAc (v/v)=1/3) to give the title compound as a yellow solid (290 mg, 70.6%).

WORKUP

后处理

  1. temperaturewarmed up to rt
  2. stirringto stir for 3 hours
  3. concentrationThe mixture was concentrated in vacuo
  4. customthe residue was purified by a silica gel column chromatography (PE/EtOAc (v/v)=1/3)