HRID1457998

反应详情

EQUATION

反应方程式

HRID 1457998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 732 mg (2.28 mmol) of ethyl hydrogen (1-benzyloxycarbonyl-3-azetidinyl)malonate dissolved in 70 ml of acetonitrile were added 1.05 g (5.67 mmol) of Eshenmoser's salt and a catalytically effective amount of potassium acetate, followed by 4.5 hours of heating under reflux. After evaporation of the solvent, the resulting residue was mixed with 100 ml of ethyl acetate, washed with 10% citric acid aqueous solution, 10% sodium sulfite aqueous solution and saturated brine in that order, and then dried over anhydrous sodium sulfate. By evaporating the solvent, 569 mg (86%) of the title compound was obtained.

WORKUP

后处理

  1. additionwere added 1.05 g (5.67 mmol) of Eshenmoser's salt
  2. temperatureof heating
  3. temperatureunder reflux
  4. customAfter evaporation of the solvent
  5. additionthe resulting residue was mixed with 100 ml of ethyl acetate
  6. washwashed with 10% citric acid aqueous solution, 10% sodium sulfite aqueous solution and saturated brine in that order
  7. dry with materialdried over anhydrous sodium sulfate
  8. customBy evaporating the solvent