HRID1294468

反应详情

EQUATION

反应方程式

HRID 1294468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

8.0 g (33.3 mmol) 4-(1-benzylpiperidin-3-yliden)-butyronitrile are dissolved in 80 ml ethanol and added to a spatula tip of Raney-Nickel. The mixture is stirred at ca. 50° C. under hydrogen atmosphere until consumption of the theoretischen amount of hydrogen to be taken up (ca. 5 days). The mixture is filtrated from the catalyst and the solvent is removed under vacuum. The residue is chromatographically purified twice over silica gel with CHCl3/CH3OH/NH4OH (90/10/1). After drawing off the solvent, a colorless oil remains which is further processed without additional purification. Yield: 3.9 g (47%).

WORKUP

后处理

  1. custom(ca. 5 days)
  2. filtrationThe mixture is filtrated from the catalyst
  3. customthe solvent is removed under vacuum
  4. customThe residue is chromatographically purified twice over silica gel with CHCl3/CH3OH/NH4OH (90/10/1)
  5. customa colorless oil remains which is further processed without additional purification