반응 #1764231

ord-44c3cae7c33c4a8dbdaf57a88c9e8abd

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction was heated at 60° C. until reaction complete by LCMS
  2. 2
    workup.ADDITIONwas added cautiously to neutral pH (Effervescence)
  3. 3
    여과the slurry was filtered
  4. 4
    기타the filtrate evaporated
  5. 5
    기타the resulting residue was used without further purification

실험 절차

Concentrated Sulfuric acid (1.0 mL, 18.8 mmol) was added to tert-butyl 4-oxo-3-(2-oxo-1,2-dihydropyridin-3-yl)piperidine-1-carboxylate (350 mg, 1.20 mmol). The resulting thick solution was stirred at room temperature overnight. The reaction was heated at 60° C. until reaction complete by LCMS. The reaction was diluted with 90% Acetonitrile 10% Water and solid potassium carbonate was added cautiously to neutral pH (Effervescence), the slurry was filtered and the filtrate evaporated, the resulting residue was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08008279B2uspto-grants-2011_08