HRID42593
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
PROCEDURE
实验过程
To a solution of 4,6-bis(4-fluorophenyl)-2-(2-phthalimidoethyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridine (0.09 g, 0.2 mmol, obtained in example 89) in EtOH (2 mL), hydrazine monohydrate (0.02 g, 0.3 mmol) was added and the mixture was heated to reflux for 3 h. A mixture of water and EtOAc was added. The phases were separated. The aqueous phase was extracted with EtOAc. The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using CHCl3-MeOH mixtures of increasing polarity as eluent, to afford 57 mg of the title compound (yield: 83%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureto reflux for 3 h
- additionwas added
- customThe phases were separated
- extractionThe aqueous phase was extracted with EtOAc
- dry with materialThe organic phase was dried over Na2SO4
- concentrationconcentrated to dryness
- customThe crude product obtained
- customwas purified by chromatography on silica gel
- temperatureof increasing polarity as eluent