Reaktion #84553

ord-6f7369845df74bf493cc21caae373ac3

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was cooled to 0° C.
  2. 2
    Extraktionextracted with DCM (20 mL×2)
  3. 3
    WaschenThe combined organic layers were washed with brine (20 mL×2)
  4. 4
    Trocknendried over anhydrous Na2SO4
  5. 5
    Einengenconcentrated in vacuo

Vorschrift

To a solution of KOH (2.38 g, 42.4 mmol) in mixed solvents of water (50 mL) and ethanol (70 mL) was added ethyl-2-(3-fluorophenoxy)-2-methylpropanoate (3.20 g, 14.1 mmol) in one portion and the mixture was stirred at 40° C. for 2 h. The mixture was cooled to 0° C., acidified to pH 3 with concentrated hydrochloric acid and extracted with DCM (20 mL×2). The combined organic layers were washed with brine (20 mL×2), dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound as a white solid (1.70 g, 61%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434695B2uspto-grants-2016_09