Reaktion #1478520

ord-19b9f76e796a4b278719148d0a15ce32

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with chloroform
  2. 2
    WaschenThe chloroform solution was washed with 10% NaHCO3 solution (100 ml)
  3. 3
    Trocknendried (MgSO4)
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigeevaporated

Vorschrift

Aluminium chloride (0.6 g, 0.004 mole) was stirred in dichloromethane (2 ml) and treated with 4-trifluoromethylbenzoyl chloride (1 g, 0.0048 mole) (ice-bath cooling) and then with 4-ethylanisole (0.6 g, 0.0044 mole) in dichloromethane (1 ml). The mixture was stirred at room temperature overnight and then poured into ice and concentrated hydrochloric acid and extracted with chloroform. The chloroform solution was washed with 10% NaHCO3 solution (100 ml), dried (MgSO4), filtered and evaporated to leave 5-ethyl-2-methoxy-4'-trifluoromethylbenzophenone (1.2 g) as a yellow oil. The latter was heated in 55% aqueous hydrogen bromide (27.5 ml) at 110°-120° C. for 5 hours. The mixture was evaporated to dryness to leave the required product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04141995uspto-grants-1979_02