HRID476203

反应详情

EQUATION

反应方程式

HRID 476203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThen, the reaction solution was concentrated by distillation under reduced pressure, and ethyl acetate (5 mL) and water (5 mL)
  2. additionwere added
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customseparated by column chromatography (n-Hex/EtOAc=10/1 (v/v))