HRID870451
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewarmed up to rt
- stirringstirred for 12 hours
- concentrationThe mixture was concentrated in vacuo
- customthe residue was purified by a silica gel column chromatography (DCM/CH3OH (v/v)=20/1)