반응 #1056846
ord-1c1a2b8012e747229cfa1d19629dbef4
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도was heated
- 2온도the mixture was heated
- 3온도at reflux for 10 min
- 4기타evaporated
- 5workup.ADDITIONThe residue was mixed with CH2Cl2
- 6세척washed with H2O twice
- 7건조The organic layer was dried over Na2SO4
- 8기타evaporated under reduced pressure
- 9기타The 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.