Reaktion #4377

ord-986aa5b3e849477ab861a73561ebea06

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe silver iodide was removed by filtration
  2. 2
    Waschenwashed with acetic acid
  3. 3
    SonstigeThe filtrate was partitioned between ether and water
  4. 4
    WaschenThe ether layer was washed with water, sodium bicarbonate solution and sodium thiosulfate solution
  5. 5
    TrocknenThe ether solution was dried with MgSO4
  6. 6
    Sonstigeevaporated to dryness in vacuo

Vorschrift

Samples of iodine (42.4 g, 0.167 mole) and silver acetate (27.87 g, 0.167 mole) were added in portions to a solution of 29.8 g (0.167 mole) of 1-(3-methoxyphenyl)butane-3-one in 167 ml of glacial acetic acid. The mixture was stirred one hour. The silver iodide was removed by filtration and washed with acetic acid. The filtrate was partitioned between ether and water. The ether layer was washed with water, sodium bicarbonate solution and sodium thiosulfate solution. The ether solution was dried with MgSO4 and evaporated to dryness in vacuo. There was obtained 41.8 g (82% yield) of oily 1-(2-iodo-5-methoxyphenyl)butane-3-one.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04725602uspto-grants-1988_02