반응 #44987

ord-3cfdcd3ae1cd4dcda832ba6fde1a4899

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling
  2. 2
    농축concentrated under reduced pressure
  3. 3
    workup.ADDITIONWater and chloroform are poured to the residue, and aqueous layer
  4. 4
    workup.ADDITIONis acidified by addition of 2 N hydrochloric acid
  5. 5
    기타The organic layer is separated
  6. 6
    세척washed with saturated brine
  7. 7
    건조dried over sodium sulfate
  8. 8
    기타The solvent is removed by evaporation under reduced pressure

실험 절차

t-Butyl 4-[trans-4-(methoxycarbonyl)cyclohexyl]-3-oxopiperazine-1-carboxylate (385 mg) obtained in Reference Example 71 (3) is dissolved in methanol (8 ml), and thereto is added 1 N aqueous sodium hydroxide solution (3.4 ml) under ice-cooling. The reaction solution is stirred at room temperature for 20 hours and concentrated under reduced pressure. Water and chloroform are poured to the residue, and aqueous layer is acidified by addition of 2 N hydrochloric acid. The organic layer is separated, washed with saturated brine and dried over sodium sulfate. The solvent is removed by evaporation under reduced pressure to give the title compound (375 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737161B2uspto-grants-2010_06