HRID522153

反应详情

EQUATION

反应方程式

HRID 522153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of potassium (Z)-1-cyano-3-ethoxy-3-oxoprop-1-en-2-olate (3.73 g, 20.82 mmol) in ethanol (100 mL) was added (3-(benzyloxy)phenyl)hydrazine hydrochloride (Preparation 61, 5.22 g, 20.82 mmol) and the reaction was heated at reflux for 24 hours. The reaction was cooled to room temperature, the solid was filtered and the filtrate was concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 20-40% EtOAc in heptanes to afford the title compound (4.76 g, 68%).

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. temperatureat reflux for 24 hours
  3. filtrationthe solid was filtered
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe residue was purified
  6. washeluting with 20-40% EtOAc in heptanes