Reaktion #649985

ord-318d15367aa34fcba8f7f753ed46ab7a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    ExtraktionThe aqueous phase is extracted with ether
  2. 2
    Extraktionthe combined organic phases extracted with 2N HCI and saturated aqueous NaCI
  3. 3
    workup.ADDITIONThe organic phase is further treated with activated charcoal, magnesium sulphate
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigethe solvent removed in vacuo

Vorschrift

1,2-Diethylbenzene (10.9 g, 74.6 mmol) and propionyl chloride (9.7 g, 74.6 mmol) are added dropwise to AlCl3 (22.3 g, 167.8 mmol) in nitromethane (75 mL) over 30 min. The reaction mixture is stirred at room temperature for 2 hours, after which 70 g of ice and 14 mL concentrated sulphuric acid are added. The aqueous phase is extracted with ether, and the combined organic phases extracted with 2N HCI and saturated aqueous NaCI. The organic phase is further treated with activated charcoal, magnesium sulphate, and filtered, and the solvent removed in vacuo.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08067437B2uspto-grants-2011_11