HRID2191144

反应详情

EQUATION

反应方程式

HRID 2191144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1.6 g (4.7 mmol) 1-[(3S,4S)-1-Benzyl-3-(4-chloro-phenyl)-piperidin-4-yl]-ethanone oxime in 300 mL methanol was hydrogenated over Raney Nickel (3.5 bar, 30° C., 23 h). The mixture was filtered and evaporated to dryness. The residue was purified by column chromatography over silica eluting with a gradient formed from DCM, methanol and NH3aq. to yield after evaporation of the product containing fractions 0.7 g (45%) of the title compound as colorless viscous oil. MS (m/e): 329.4 [(M+H)+].

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customevaporated to dryness
  3. customThe residue was purified by column chromatography over silica eluting with a gradient
  4. customformed from DCM, methanol and NH3aq
  5. customto yield
  6. customafter evaporation of the product
  7. additioncontaining fractions 0.7 g (45%) of the title compound as colorless viscous oil