반응 #6891

ord-0a730dd69aee4455b345209e15cac609

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도at reflux for 4 h
  3. 3
    기타the solvent removed under vacuum
  4. 4
    기타The mixture was transferred to a separatory funnel
  5. 5
    세척washed with water (3×15 mL)
  6. 6
    건조The organic layer was dried over sodium sulfate
  7. 7
    여과filtered
  8. 8
    기타the solvent removed under vacuum

실험 절차

The product (208 mg, 1.0 mmol) from Step B and piperidine (0.5 mL, 5 mmol) were mixed in absolute ethanol (3 mL) and then heated at reflux for 4 h. The reaction mixture was cooled to r.t., and the solvent removed under vacuum. The solids were taken up in EtOAc (125 mL). The mixture was transferred to a separatory funnel and washed with water (3×15 mL). The organic layer was dried over sodium sulfate, filtered and the solvent removed under vacuum to afford the product as a yellow solid, MS: m/z 258 (MH+) which was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084156B2uspto-grants-2006_08