Reaktion #89367

ord-4705ada6d96d46f0b0f74ced5f46e5bb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux overnight
  2. 2
    SonstigeThe solvent was removed in vacuo
  3. 3
    Sonstigeto obtain the crude which
  4. 4
    Sonstigewas purified by silica gel chromatography (0˜100% DCM/EtOAc)

Vorschrift

6-Methyl-3-(1H-pyrazol-1-yl)picolinonitrile (0.60 g, 3.26 mmol) and NaOH (1.37 g, 34.2 mmol) were dissolved in methanol (3 mL) and stirred at reflux overnight. The reaction was cooled to rt, diluted with more methanol (5 mL), and acidified with AcOH to pH 4-5. The solvent was removed in vacuo to obtain the crude which was purified by silica gel chromatography (0˜100% DCM/EtOAc) to yield the title compound as a clear oil (0.62 g, 94%). MS (ESI) 204 (M+H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440982B2uspto-grants-2016_09