HRID1639381

反应详情

EQUATION

反应方程式

HRID 1639381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.00 g (0.006 mol) of 2-(4-acetamidobutyryl)-5-chlorohydrocinnamic acid and 0.5 ml (0.006 mol) of thionyl chloride in 20 ml of methylene chloride are stirred at room temperature for 5 minutes and then a solution of 2.2 ml (0.023 mol) of 3-hydroxymethylpyridine in 20 ml of methylene chloride is added thereto at 0°. After stirring at room temperature for 1 hour, the solution is concentrated, extracted with methylene chloride/water, dried with magnesium sulfate and the solvent is distilled in a vacuum. Chromatography on aluminum oxide with ethyl acetate gives 3-pyridylmethyl 2-(4-acetamidobutyryl)-5-chlorohydrocinnamate as a beige oil.

WORKUP

后处理

  1. customat 0°
  2. concentrationthe solution is concentrated
  3. extractionextracted with methylene chloride/water
  4. dry with materialdried with magnesium sulfate
  5. distillationthe solvent is distilled in a vacuum