Reaktion #742984

ord-8d8961b4498f45c493c8ac48ba937f36

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled in an ice-bath (above f.p)
  2. 2
    Sonstigeto come to rt
  3. 3
    SonstigeReaction mixture
  4. 4
    Temperaturwas cooled
  5. 5
    FiltrationThe resulting yellow solid was filtered
  6. 6
    Waschenwashed with ice-water
  7. 7
    Sonstigedried

Vorschrift

Fuming nitric acid (83.3 mL) (>90%) was added slowly to a solution of 2,6-dimethyl bromobenzene (27.9 g, 150 mmol) in acetric acid (167 mL) and cooled in an ice-bath (above f.p). The mix was allowed to come to rt and later heated at 80° C. for 2 h. (HPLC showed no SM). Reaction mixture was cooled and poured into ice-water with stirring. The resulting yellow solid was filtered, washed with ice-water and dried to give 28.7 g of an yellow solid which was used as such in the next step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08071609B2uspto-grants-2011_12