HRID870428

反应详情

EQUATION

反应方程式

HRID 870428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 4-(4-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)-2,5-difluorophenoxy)picolinamide (80 mg, 0.17 mmol) in EtOAc (2 mL), CH3CN (2 mL), and H2O (1 mL) was added PhI(OAc)2 (70 mg, 1.2 mmol). The reaction was stirred at 0° C. for 30 minutes, then warmed up to rt and continued to stir for 8 hours. The mixture was filtered through a CELITE® pad, which was washed with EtOAc (30 mL). The filtrate was concentrated in vacuo and the residue was purified by a silica gel column chromatography (DCM/CH3OH (v/v)=20/1) to afford the tile compound as a white solid (51 mg, 68%).

WORKUP

后处理

  1. temperaturewarmed up to rt
  2. stirringto stir for 8 hours
  3. filtrationThe mixture was filtered through a CELITE® pad, which
  4. washwas washed with EtOAc (30 mL)
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue was purified by a silica gel column chromatography (DCM/CH3OH (v/v)=20/1)