반응 #1056846

ord-1c1a2b8012e747229cfa1d19629dbef4

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도the mixture was heated
  3. 3
    온도at reflux for 10 min
  4. 4
    기타evaporated
  5. 5
    workup.ADDITIONThe residue was mixed with CH2Cl2
  6. 6
    세척washed with H2O twice
  7. 7
    건조The organic layer was dried over Na2SO4
  8. 8
    기타evaporated under reduced pressure
  9. 9
    기타The residue was purified by column chromatography

실험 절차

A mixture of 2-amino-N-{4-[1-methyl-1-(1-methyl-piperidin-4-yl)ethyl]phenyl}benzamide (600 mg, Step B) and 4-pyridinecarboxaldehyde (0.22 mL) was heated at reflux in EtOH (50 mL) overnight. NaBH4 (250 mg) was added and the mixture was heated at reflux for 10 min and evaporated. The residue was mixed with CH2Cl2 and washed with H2O twice, followed by brine. The organic layer was dried over Na2SO4 and evaporated under reduced pressure. The residue was purified by column chromatography using 10% MeOH/CH2Cl2 to provide the title compound. MS (ES+): 443 (M+H)+. Calc'd. for C28H34N4O-442.27.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07307088B2uspto-grants-2007_12