HRID922259

反应详情

EQUATION

反应方程式

HRID 922259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

To a 100 mL RB flask fitted with magnetic stirrer was charged with piperidine (0.108 g, 0.13 mL, 1.35 mmol) and acetic acid (0.081 g, 0.08 mL, 1.35 mmol). To this, toluene (20 mL) was added, followed by 4-(benzyloxy)-2-methoxybenzaldehyde (1.1 g, 4.5 mmol) and diethyl malonate (0.87 g, 5.5 mmol). The RM was heated at 125° C., by fitted with a dean-stark's apparatus for 5 h. After 5 h, the RM was concentrated; water (50 mL) was added and extracted with ethyl acetate (50 mL×2)). The organic layer was washed with saturated brine solution (50 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The product was obtained as yellow solid. (0.775 g, yield: 44.2%).

WORKUP

后处理

  1. customTo a 100 mL RB flask fitted with magnetic stirrer
  2. customby fitted with a dean-stark's apparatus for 5 h
  3. concentrationthe RM was concentrated
  4. additionwater (50 mL) was added
  5. extractionextracted with ethyl acetate (50 mL×2))
  6. washThe organic layer was washed with saturated brine solution (50 mL)
  7. dry with materialThe organic layer was dried over anhydrous Na2SO4
  8. customthe solvent was removed under reduced pressure
  9. customThe product was obtained as yellow solid