Reaktion #664802

ord-201b88bf6fc740fa8390e2decb1b2841

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 HCl and saturated aqueous NaCl
  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 HCl and saturated aqueous NaCl. 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: US09040559B2uspto-grants-2015_05