反应 #428989

ord-8b842faff5664f7eb8d5b8b7e1f54adc

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤After filtration of the catalyst
  2. 2
    其他through cellite and evaporation of the solvent
  3. 3
    workup.ADDITIONTherefore 0.6 g of Pearlman's catalyst was added in 40 ml ethanol (95%) once more
  4. 4
    workup.ADDITIONthe mixture was treated under H2 -atmosphere at 0.28 MPa over night
  5. 5
    过滤Filtration
  6. 6
    其他through cellite and evaporation of the solvent
  7. 7
    其他gave the product in a quantitative yield (2.18 g)

实验过程

3.1 g (0.01 mol) (3RS)-1-benzyl-3-(N-tert-butyloxycarbonylaminoethyl) pyrrolidine was hydrogenated at 0.28 MPa over 0.6 g of Pearlman's catalyst (Pd(OH)2) in 40 ml ethanol (95%) over night. After filtration of the catalyst through cellite and evaporation of the solvent 1H-NMR showed that the reaction was not completed. Therefore 0.6 g of Pearlman's catalyst was added in 40 ml ethanol (95%) once more and the mixture was treated under H2 -atmosphere at 0.28 MPa over night. Filtration through cellite and evaporation of the solvent gave the product in a quantitative yield (2.18 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05856307uspto-grants-1999_01