Reaktion #623015

ord-1e3e9aa2b7f645eb888aa5eb14441c43

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction was refluxed overnight
  2. 2
    Sonstigepartitioned with water
  3. 3
    SonstigeThe organic layer was separated
  4. 4
    Extraktionthe aqueous layer was extracted with CH2Cl2
  5. 5
    WaschenThe combined organic extracts were washed with water
  6. 6
    Trocknendried over Na2SO4
  7. 7
    Filtrationfiltered
  8. 8
    Einengenconcentrated
  9. 9
    Sonstigeto afford the material that
  10. 10
    Sonstigewas not purified

Vorschrift

Into a solution of 1-methyl-4-nitro-2-trifluormethylbenzene (4.1 g, 20 mmol) in carbon tetrachloride (30 mL) were added NBS (5.4 g, 30 mmol) and AIBN (493 mg, 3 mmol). The reaction was refluxed overnight and then partitioned with water. The organic layer was separated and the aqueous layer was extracted with CH2Cl2. The combined organic extracts were washed with water, dried over Na2SO4, filtered and concentrated to afford the material that was not purified but used directly in the next step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08859553B2uspto-grants-2014_10