Reaktion #7593

ord-aeca40a5c11b49e09fe5ba429ff41801

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    ExtraktionAfter extraction with ethyl acetate
  2. 2
    Waschenthe organic layer was washed with water
  3. 3
    Trocknenbrine, dried (MgSO4)
  4. 4
    Sonstigethe solvent evaporated
  5. 5
    FiltrationThe solid was filtered off
  6. 6
    Waschenwashed with hexane
  7. 7
    Sonstigedried under vacuum

Vorschrift

The starting material 5-benzyloxy-2-fluoro-4-methylnitrobenzene was obtained by adding benzyl bromide (3 ml, 25 mmol) to a solution of 2-fluoro-5-hydroxy-4-methylnitrobenzene (3.92 mg, 23 mmol) in DMF (70 ml) containing potassium carbonate (9.5 g, 68 mmol). After stirring for 3 hours at 60° C. the mixture was diluted with water and adjusted to pH2. After extraction with ethyl acetate, the organic layer was washed with water and then brine, dried (MgSO4) and the solvent evaporated. The solid was filtered off, washed with hexane and dried under vacuum to give 5-benzyloxy-2-fluoro-4-methylnitrobenzene (4.83 g, 80%).

Quelle

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