HRID747006

反应详情

EQUATION

反应方程式

HRID 747006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Palladium on carbon (5%, 800 mg) was added to a solution of 1,1-dimethylethyl 4-hydroxy-4-(3-hydroxypropynyl)-1-piperidinecarboxylate (from step (ii) above; 8.37 g, 32.8 mmol) in ethanol (400 ml), acetic acid (40 ml) and water (5 ml) and the mixture was shaken under an atmosphere of hydrogen (40 psi) for 20 hours. The mixture was filtered through Hyflo™ and the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with isohexane/EtOAc (50:50 increasing to 0:100), to give the title compound (4.84 g, 57%).

WORKUP

后处理

  1. filtrationThe mixture was filtered through Hyflo™
  2. customthe solvent was evaporated under reduced pressure
  3. customThe residue was purified by flash column chromatography on silica gel
  4. washeluting with isohexane/EtOAc (50:50 increasing to 0:100)