反応 #964

ord-2326e4f1e4844936a51646b96ee23d0d

反応方程式

CC(C)(C)OC(=O)NCCC1CCN(Cc2ccccc2)C1
(3RS)-1-benzyl-3-(N-tert-butyloxycarbonylaminoethyl) pyrrolidine
CC(C)(C)OC(=O)NCCC1CCNC1
(3RS)-3-(N-tert-butyloxycarbonylaminoethyl) pyrrolidine

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過After filtration of the catalyst
  2. 2
    その他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
    ろ過Filtration
  6. 6
    その他through cellite and evaporation of the solvent
  7. 7
    その他gave the product in a quantitative yield (2.18 g)

実験手順

3.1 g (0.0t 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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723444uspto-grants-1998_03