HRID476203
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
- 60 °C
PROCEDURE
实验过程
2-hydrazinopyridine (161 mg, 1.477 mmol) was added to a solution of (E)-ethyl-5-phenyl-3-oxopent-4-enoate (8a, 355 mg, 1.62 mmol) prepared in Example C-1 in acetic acid (3 mL), followed by stirring under reflux at 60° C. for 30 minutes. Then, the reaction solution was concentrated by distillation under reduced pressure, and ethyl acetate (5 mL) and water (5 mL) were added thereto, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and separated by column chromatography (n-Hex/EtOAc=10/1 (v/v)) to afford the title compound.
WORKUP
后处理
- concentrationThen, the reaction solution was concentrated by distillation under reduced pressure, and ethyl acetate (5 mL) and water (5 mL)
- additionwere added
- extractionfollowed by extraction with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- customseparated by column chromatography (n-Hex/EtOAc=10/1 (v/v))