HRID563445
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
A mixture of (4-hydroxy-1-phenyl-1H-pyrazolo[3,4-b]pyridin-5-yl)(phenyl)methanone (0.38 g, 1.2 mmol) and phosphorus oxychloride (1.3 mL) was stirred at 110° C. for 1.5 hr. The mixture was cooled, poured onto ice, basified with sodium hydroxide aqueous solution to pH=8, and extracted with ethyl acetate. Combined extracts were dried (Na2SO4) and concentrated. Flash chromatography gave (4-chloro-1-phenyl-1H-pyrazolo[3,4-b]pyridin-5-yl)(phenyl)methanone (0.26 g, 0.79 mmol, 66% yield) as a yellow solid.
WORKUP
后处理
- temperatureThe mixture was cooled
- additionpoured onto ice
- extractionextracted with ethyl acetate
- dry with materialCombined extracts were dried (Na2SO4)
- concentrationconcentrated