Reaktion #515991

ord-f92490fc3a8945b38c23a47081af8dc9

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONare added
  2. 2
    Extraktionthe ether phase is extracted
  3. 3
    Waschenby washing several times with water and saturated sodium chloride solution
  4. 4
    Trocknendried over sodium sulfate
  5. 5
    Sonstigethe solvent is evaporated off
  6. 6
    workup.DISTILLATIONDistillation at 150° C. (0.01 mbar)

Vorschrift

30 g of 1-(4-hydroxyphenyl)-propan-2-one and 45.5 g of chloromethyl-dimethyl-(4-fluorophenyl)-silane in 400 ml of dimethyl sulfoxide are stirred with 42 g of potassium carbonate and 2 g of potassium iodide for 12 hours at 70° C. The reaction mixture is poured into 1.6 liters of ice water and 500 ml of diethyl ether are added; the ether phase is extracted by washing several times with water and saturated sodium chloride solution and dried over sodium sulfate; the solvent is evaporated off. Distillation at 150° C. (0.01 mbar) yields the title product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06313344B1uspto-grants-2001_11