Reaktion #415354

ord-bfd9fc9767ed4168b6b660882cce32be

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling in an ice-bath
  2. 2
    Sonstigethe temperature below 5°
  3. 3
    workup.ADDITIONAfter addition
  4. 4
    workup.STIRRINGthe product is stirred for another hour before hydrolyzing
  5. 5
    workup.STIRRINGwith stirring
  6. 6
    WaschenThe organic phase is washed with successive portions of dilute hydrochloric acid, sodium carbonate, and water
  7. 7
    workup.DISTILLATIONdistilled

Vorschrift

To a suspension of anhydrous aluminum chloride (467 g,; 3.5 moles) in carbon tetrachloride (2 l.) is added acetyl chloride (275 g.; 249 cc., 3.5 moles) during 15 minutes with vigorous stirring and cooling in an ice-bath. Cyclohexylbenzene (481 g.; 3.0 moles) is added dropwise over a period of 3 hours, keeping the temperature below 5°. After addition is complete, the product is stirred for another hour before hydrolyzing by pouring into ice and hydrochloric acid with stirring. The organic phase is washed with successive portions of dilute hydrochloric acid, sodium carbonate, and water, and distilled to give p-cyclohexylacetophenone, (b.p. 88°-95.5°/ 0.05 mm.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04016214uspto-grants-1977_04