Reaktion #63695

ord-6a1d1b7f41cc4078a574d6eee7881fa9

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    workup.ADDITIONAfter complete addition
  2. 2
    TemperaturThe mixture was cooled
  3. 3
    ExtraktionThe resultant mixture was extracted with ethyl acetate
  4. 4
    Waschenthe extract was washed with a 1N sodium hydroxide solution
  5. 5
    ExtraktionThe washed extract
  6. 6
    Trocknenwas dried over anhydrous magnesium sulfate
  7. 7
    Filtrationwas filtered
  8. 8
    SonstigeThe solvent was evaporated under reduced pressure

Vorschrift

To a stirred solution of 15.8 g (0.083 mole) of 2-chloro-4-fluoro-5-nitrophenol in 90 mL of acetone was added 17.1 g (0.12 mole) of potassium carbonate followed by a solution of 21.0 g (0.12 mole) of 2-iodopropane in 10 mL of acetone. After complete addition, the reaction mixture was heated at 60° C. for approximately 18 hours. The mixture was cooled and poured into a mixture of ice and concentrated hydrochloric acid. The resultant mixture was extracted with ethyl acetate, and the extract was washed with a 1N sodium hydroxide solution. The washed extract was dried over anhydrous magnesium sulfate and was filtered. The solvent was evaporated under reduced pressure to leave 17.7 g of 4-chloro-2-fluoro-5-(1-methylethoxy)nitrobenzene as a solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04766233uspto-grants-1988_08