HRID520679

反应详情

EQUATION

反应方程式

HRID 520679 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 solution of 4-((6-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)pyridin-3-yl)oxy)picolinamide (111 mg, 0.25 mmol) in EtOAc (2 mL), CH3CN (2 mL) and H2O (1 mL) was added PhI(OAc)2 (97 mg, 0.3 mmol). The reaction was stirred at 0° C. for 30 minutes, then warmed up to rt and further 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)=40/1) to give the title compound as a light beige solid (85 mg, 81.7%).

WORKUP

后处理

  1. temperaturewarmed up to rt
  2. stirringfurther stirred 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)=40/1)