Reaktion #7577

ord-994883380a214f47b45d3a084572d5ee

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 4 hours
  3. 3
    Temperaturto cool
  4. 4
    Extraktionextracted with ethyl acetate (100 ml)
  5. 5
    ExtraktionThe ethyl acetate extract
  6. 6
    Trocknenwas dried (MgSO4)
  7. 7
    Sonstigethe solvent removed by evaporation

Vorschrift

A mixture of 4-fluoro-2-methyl-5-nitrophenol (2.1 g, 13 mmol), iron powder (1 g, 18 mmol) and iron(II)sulphate (1.5 g, 10 mmol) in water (40 ml) was heated at reflux for 4 hours. The reaction mixture was allowed to cool, neutralised with 2M aqueous sodium hydroxide solution and extracted with ethyl acetate (100 ml). The ethyl acetate extract was dried (MgSO4) and the solvent removed by evaporation to give 2-fluoro-5-hydroxy-4-methylaniline (0.8 g, 47%) as a solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087602B2uspto-grants-2006_08