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
- 100 °C
PROCEDURE
实验过程
A solution of 4-chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline (1.47 g, 5.00 mmol), morpholine (0.87 g, 10.0 mmol) and potassium carbonate (1.38 g, 10.0 mmol) in N,N-dimethylformamide (20 mL) was heated under reflux at 100° C. for 12 hours. The solution was cooled to room temperature, and concentrated under reduced pressure. The residue was poured into water and organic matter was extracted with chloroform. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and evaporated under reduced pressure. The residue thus obtained was purified by basic silica gel column chromatography (hexane:chloroform=3:1) to give the title compound (0.63 g, 36% yield).
WORKUP
后处理
- temperatureThe solution was cooled to room temperature
- concentrationconcentrated under reduced pressure
- additionThe residue was poured into water and organic matter
- extractionwas extracted with chloroform
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customevaporated under reduced pressure
- customThe residue thus obtained
- customwas purified by basic silica gel column chromatography (hexane:chloroform=3:1)