Reaktion #1552191

ord-bb1bce41eaf74230ab1a9d19073fc347

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    EinengenThe reaction mixture was concentrated
  3. 3
    workup.ADDITIONa mixed solvent (DCM/MeOH=5/1) was added
  4. 4
    FiltrationThe remaining solid was filtered
  5. 5
    Einengenthe filtrate was concentrated

Vorschrift

Methyl 4-(1-methylpiperidine-4-yloxy)-3-(trifluoromethyl)benzoate (512 mg, 1.61 mmol) was dissolved in a mixture of THF (1.5 mL), MeOH (1.5 mL) and H2O (1.5 mL), and then NaOH (193 mg, 4.84 mmol) was added thereto. The reaction mixture was stirred at 90° C. for 22 hours and cooled to room temperature, and 1N HCl was added dropwise thereto to pH 4. The reaction mixture was concentrated, and a mixed solvent (DCM/MeOH=5/1) was added thereto. The remaining solid was filtered, and the filtrate was concentrated to obtain the title compound (391 mg, 80%) without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08999973B2uspto-grants-2015_04