Reaktion #583814

ord-62404d69730a4060a8d31770412df45f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter 2 hrs the reaction mixture was evaporated
  2. 2
    Sonstigeto remove the methanol
  3. 3
    Sonstigepartitioned between ethyl ether (20 mL) and 2N aqueous sodium hydroxide solution (20 mL)
  4. 4
    Extraktionextracted with ethyl acetate(3×20 mL)
  5. 5
    WaschenThe combined organics were washed with water (20 mL) and brine (20 mL)
  6. 6
    Filtrationfiltered through phase
  7. 7
    Sonstigeseparating paper
  8. 8
    Sonstigeevaporated

Vorschrift

2N Aqueous sodium hydroxide solution (2.0 mL, 4 mmol) was added to a solution of compound (28) (2.06 mmol) in methanol (10 mL) at ambient temperature. After 2 hrs the reaction mixture was evaporated to remove the methanol and then partitioned between ethyl ether (20 mL) and 2N aqueous sodium hydroxide solution (20 mL). The aqueous phase was acidified to pH⅔ with 2N HCl and extracted with ethyl acetate(3×20 mL). The combined organics were washed with water (20 mL) and brine (20 mL), filtered through phase separating paper and evaporated to yield 2-benzyl-4nitrobenzoic acid (compound 29).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06946468B1uspto-grants-2005_09