HRID479525

反应详情

EQUATION

反应方程式

HRID 479525 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-chlorobenzamide (1.50 g, 9.6 mmol), propionaldehyde diethyl acetal (1.53 g, 11.6 mmol), and benzotriazole (1.15 g, 9.6 mmol) in toluene (35 mL) was treated with p-toluenesulfonic acid (100 mg, 0.53 mmol). The mixture was heated at reflux under Dean-Stark conditions for 16 hours, cooled to ambient temperature, and concentrated to dryness. The crude material was purified by flash chromatography (elution with 40% ethyl acetate/hexanes) to provide 0.860 g of the desired product as a white solid.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux under Dean-Stark conditions for 16 hours
  3. concentrationconcentrated to dryness
  4. customThe crude material was purified by flash chromatography (elution with 40% ethyl acetate/hexanes)