Reaktion #86458

ord-66dfde43b4094517a531ba18ffed4f1b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 24 h
  2. 2
    SonstigeThe resulting reaction mixture
  3. 3
    Einengenconcentrated under vacuum
  4. 4
    Sonstigeto get a crude residue
  5. 5
    Extraktionextracted with ether (3×30 mL)
  6. 6
    FiltrationHCl and the precipitated solid was filtered
  7. 7
    Waschenwashed with cold water
  8. 8
    Sonstigedried in vacuo

Vorschrift

A suspension of methyl 2-chloro-6-fluoro-3,5-dimethoxybenzoate (2.7 g, 0.010 mol) and sodium hydroxide (1.088 g, 0.0272) in anhydrous ethanol (30 mL) was refluxed for 24 h. The resulting reaction mixture was cooled to room temperature and concentrated under vacuum to get a crude residue. The crude residue was dissolved in water and extracted with ether (3×30 mL). The aqueous layer was acidified with conc.HCl and the precipitated solid was filtered, washed with cold water and dried in vacuo to afford the title compound (1.8 g, yield: 71%) as a solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434697B2uspto-grants-2016_09