HRID1913879
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
To a solution of 6-hydroxy-3,4-dihydroquinolin-2(1H)-one (0.55 g) in acetonitrile (10 mL), cesium carbonate (2.0 g) and (2R)-1-(3-chloropropyl)-2-methylpyrrolidine prepared in Example 1-(1) (0.50 g) were added and stirred at 100° C. for 1 hour. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and the resulting residue was purified by NH-type silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=1/1). The resulting solid was subjected to recrystallization from n-hexane to give the titled compound (0.33 g, 37%) as a colorless powder.
WORKUP
后处理
- additionwere added
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customthe resulting residue was purified by NH-type silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=1/1)
- customThe resulting solid was subjected to recrystallization from n-hexane