반응 #547359

ord-acc06917dec44dd4b47cbd19ddf89510

용매

반응 조건

온도
95°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling to RT
  2. 2
    추출extracted with EtOAc (4×80 mL)
  3. 3
    세척washed with H2O (50 mL)
  4. 4
    기타The organic layer was separated
  5. 5
    건조dried over Na2SO4
  6. 6
    여과filtered
  7. 7
    농축concentrated under reduced pressure

실험 절차

To a solution of 2-bromo-6-(piperidylmethyl)pyridine (5.21 g, 20 mmol) in IpOH (30 mL) in a sealed tube at RT, a catalytic amount of Cu (100 mg) and 28–30% NH4OH (35 mL) were added. The stirred suspension was heated to 95° C. for 40 h. After cooling to RT, the reaction mixture was diluted with H2O (100 mL) and extracted with EtOAc (4×80 mL). The organic layers were combined, then washed with H2O (50 mL) followed by brine (50 mL). The organic layer was separated, dried over Na2SO4, filtered and concentrated under reduced pressure to yield the title compound as a dark yellow oil. This was used as crude. MS m/z: 193 (M+H)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07196104B2uspto-grants-2007_03