HRID2191144
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe mixture was filtered
- customevaporated to dryness
- customThe residue was purified by column chromatography over silica eluting with a gradient
- customformed from DCM, methanol and NH3aq
- customto yield
- customafter evaporation of the product
- additioncontaining fractions 0.7 g (45%) of the title compound as colorless viscous oil