Reaktion #56522

ord-dc15e23bc8184272bff1e209a9457cc9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthermometer and reflux condenser
  2. 2
    workup.ADDITIONcharged with 2.62 kg
  3. 3
    Temperaturthe batch is heated
  4. 4
    Temperaturto reflux over 2.5 hours
  5. 5
    TemperaturThe batch is refluxed for 2 hours (in solution at 75°)
  6. 6
    Temperaturcooled to 100°

Vorschrift

A 30 liter resin pot is fitted with stirrer, thermometer and reflux condenser, and charged with 2.62 kg. of 50% aqueous sodium hydroxide and 11.34 liters of water. 4-(2',4'-Difluorophenyl)phenylacetate (1.876 kg., 7.55 m) is added and the batch is heated to reflux over 2.5 hours. The batch is refluxed for 2 hours (in solution at 75°), then cooled to 100° and added to a solution of 3.27 liters of concentrated hydrochloric acid in 9.8 liters of water in a 50 liter resin pot over a 30 minute period.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04225730uspto-grants-1980_09