Reaktion #169966

ord-684f4c34193e42d59ba6b0a5c7b2c560

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe resulting mixture was heated
  2. 2
    Temperaturat reflux for 24 h
  3. 3
    TemperaturAfter cooling the solvent
  4. 4
    Sonstigewas removed in vacuo

Vorschrift

SOCl2 (4.16 g, 30.1 mmol) was added to a solution of 2,6-difluoro-4-hydroxybenzoic acid (1.50 g, 8.62 mmol) in MeOH (20 mL) and the resulting mixture was heated at reflux for 24 h. After cooling the solvent was removed in vacuo to give the title compound (1.62 g, 99%) as a white crystalline solid; mp 177.5-180° C.; 1H NMR (270 MHz, DMSO-d6) 3.80 (3H, s, CH3), 6.50-6.60 (2H, m, ArH), 11.16 (1H, s, OH)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846737B2uspto-grants-2014_09