HRID870451

反应详情

EQUATION

反应方程式

HRID 870451 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 4-(5-chloro-4-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)-2-fluorophenoxy)picolinamide (297.6 mg, 0.6 mmol) in EtOAc (4 mL), CH3CN (4 mL) and H2O (2 mL) was added PhI(OAc)2 (97 mg, 0.3 mmol) at 0° C., the mixture was stirred at 0° C. for 30 minutes, then warmed up to rt and stirred for 12 hours. The mixture was concentrated in vacuo and the residue was purified by a silica gel column chromatography (DCM/CH3OH (v/v)=20/1) to give the title compound as a light beige solid (220 mg, 78.3%).

WORKUP

后处理

  1. temperaturewarmed up to rt
  2. stirringstirred for 12 hours
  3. concentrationThe mixture was concentrated in vacuo
  4. customthe residue was purified by a silica gel column chromatography (DCM/CH3OH (v/v)=20/1)