Reaktion #66520

ord-077c9c4ea8274fb796a20617fa6ba2d7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter evaporation of EtOH
  2. 2
    Extraktionwas extracted with AcOEt
  3. 3
    WaschenThe organic phase was washed with brine
  4. 4
    Trocknenwas dried over MgSO4
  5. 5
    Filtrationwas filtered
  6. 6
    Einengenwas concentrated under reduced pressure

Vorschrift

According to Scheme 3 Step 2: A suspension of iron (5.07 mmol, 283 mg), acetic acid (1.22 mmol, 70 μL) and of 2-chloro-1-(3-chlorophenoxy)-4-nitrobenzene (1.02 mmol, 288 mg) in water/EtOH (1:1, 8 mL) was stirred at 80° C. for 30 minutes. After evaporation of EtOH, the aqueous phase was basified with a saturated solution of NaHCO3 and was extracted with AcOEt. The organic phase was washed with brine, was dried over MgSO4, was filtered and was concentrated under reduced pressure to yield 3-chloro-4-(3-chlorophenoxy)aniline (1.02 mmol, 258 mg, 100%) as a solid. The product was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524726B2uspto-grants-2013_09