반응 #963739

ord-9c7b4f4c77394b61af23fe015595cd3d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The resulting reaction mixture
  2. 2
    농축concentrated under reduced pressure
  3. 3
    workup.ADDITIONSaturated aqueous Na2CO3 was added to the resulting residue until the solution pH
  4. 4
    추출The mixture was then extracted with ethyl acetate (3×25 mL)
  5. 5
    건조The combined organic layers were dried with Na2SO4
  6. 6
    농축concentrated under reduced pressure

실험 절차

To a solution of tert-butyl 6-(pyrrolidin-1-ylmethyl)pyridin-2-ylcarbamate 82 (750 mg, 2.71 mmol) in dichloromethane (10 mL) was added trifluoroacetic acid (4.0 mL) at room temperature. The resulting reaction mixture was stirred at room temperature for 6 h and then concentrated under reduced pressure. Saturated aqueous Na2CO3 was added to the resulting residue until the solution pH reached 9. The mixture was then extracted with ethyl acetate (3×25 mL). The combined organic layers were dried with Na2SO4 and concentrated under reduced pressure to afford 49 (440 mg, 92% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08987258B2uspto-grants-2015_03