Reaktion #1715058

ord-696cb97313524e7e93da60ebfaf43c3b

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-(4-ethylphenyl)-5,6,7,8-tetrahydro[1]benzothieno[2,3-b]pyridin-3-yl]pentanoate (0.197 g; 0.468 mmol) in methanol (4.6 mL) was added a solution of sodium hydroxide 5 N (0.95 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 0.092 g (48%) of the title compound as a white solid.

Quelle

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