Reaktion #2371778

ord-218d7d80bed44409aee190f4ba5e1527

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated to dryness
  2. 2
    workup.ADDITIONdiluted the pale yellow solid with water
  3. 3
    TemperaturThe resulting semi-heterogeneous suspension was cooled in ice-bath
  4. 4
    FiltrationThe solid aggregate was collected by filtration on Buchner funnel
  5. 5
    Waschenwashed with water and suction
  6. 6
    Sonstigedried
  7. 7
    Trocknenby drying over P2O5 in a vacuum desiccator

Vorschrift

Ethyl 6-(2-(4-fluoro-3-methylphenyl)pyridin-3-yl)imidazo[1,5-a]pyridine-3-carboxylate (2.1 g) and LiOH.H2O (400 mg) were stirred in THF/H2O (1:1, 60 mL) at 70° C. for 2 h. The reaction mixture was concentrated to dryness and diluted the pale yellow solid with water. The resulting semi-heterogeneous suspension was cooled in ice-bath, stirred and neutralized with aq. 3N HCl to pH 6. The solid aggregate was collected by filtration on Buchner funnel, washed with water and suction dried. Further processing the sample by drying over P2O5 in a vacuum desiccator provided the desired 6-(2-(4-Fluoro-3-methylphenyl)pyridin-3-yl)imidazo[1,5-a]pyridine-3-carboxylic acid (1.5 g, purity: 97%) as a pale yellow solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09145433B2uspto-grants-2015_09