HRID544468

反应详情

EQUATION

反应方程式

HRID 544468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-5-benzylamino pyridine (4.0 g), triethylamine (2.1 g),3-chloro-4-oxopentanenitrile (2.7 g) and acetonitrile (50 ml) is stirred and heated under reflux for 18 hr. The solvent is removed in vacuo, and the residue is dissolved in chloroform (200 ml). The solution is washed with water (4×100 ml), dried over anhydrous potassium carbonate and the chloroform is removed in vacuo. The residue is chromatographed on silica gel (200 g) using chloroform as the eluant. The product is obtainedand crystallized from acetonitrile.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 18 hr
  3. customThe solvent is removed in vacuo
  4. dissolutionthe residue is dissolved in chloroform (200 ml)
  5. washThe solution is washed with water (4×100 ml)
  6. dry with materialdried over anhydrous potassium carbonate
  7. customthe chloroform is removed in vacuo
  8. customThe residue is chromatographed on silica gel (200 g)
  9. customThe product is obtainedand crystallized from acetonitrile