Reaktion #1715059

ord-f0dec43b7873442e8ee82fc91f363b79

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Einengenthe reaction mixture was concentrated under reduced pressure
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
  4. 4
    WaschenThe organic layer was washed with brine, water
  5. 5
    Trocknendried over magnesium sulphate
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

To a solution of methyl [2-methyl-4-(pyridin-3-yl)-5,6,7,8-tetrahydro[1]benzothieno[2,3-b]pyridin-3-yl]pentanoate (0.058 g; 0.147 mmol) in methanol (1.5 mL) was added a solution of sodium hydroxide 5 N (0.29 mL) and the mixture was heated at 60° C. for 18 h. After cooling, the reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethyl acetate and the mixture was acidified with HCl (1N) until pH 1. The organic layer was washed with brine, water, dried over magnesium sulphate and concentrated under reduced pressure to furnish 0.023 g (42%) of the title compound as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08785638B2uspto-grants-2014_07