반응 #44099

ord-966ccbaf97cf4e198a4ec66239090793

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축then concentrated
  2. 2
    workup.ADDITIONWater (30 vol) was added
  3. 3
    추출the solution was extracted with ethyl acetate (3×20 vol)
  4. 4
    추출then extracted with dichloromethane (5×40 vol)
  5. 5
    기타The combined organic extracts were dried
  6. 6
    기타evaporated

실험 절차

To a solution of 1,1-dimethylethyl 4-(2-methyl-5-quinolinyl)-1-piperazinecarboxylate in 2-propanol (3 vol) was added dropwise hydrochloric acid (37%, 3 vol). The mixture was stirred at 40° C. for 1.5 hours then concentrated. Water (30 vol) was added and the solution was extracted with ethyl acetate (3×20 vol). The aqueous layer was basified with an aqueous sodium carbonate solution then extracted with dichloromethane (5×40 vol). The combined organic extracts were dried and evaporated to give the title compound as an off-white solid (80% th, 2 steps).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732600B2uspto-grants-2010_06