Reaktion #93539

ord-3b7073b3151c4a99bac17ba77a9f95d0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water and saturated saline
  2. 2
    Trocknendried over magnesium sulfate
  3. 3
    workup.DISTILLATIONthe solvent was then distilled off
  4. 4
    SonstigeThe crude product thus obtained
  5. 5
    Sonstigewas purified by a silica gel column chromatography

Vorschrift

To a solution of 600 mg of β-(p-chlorophenyl)-α-methylene-γ-butyrolactone in 10 ml of toluene were added 0.44 ml of thiobenzoic acid and one drop of triethylamine and the reaction was effected at room temperature for 18 hours. The reaction mixture was diluted with 100 ml of ethyl ether, washed with water and saturated saline, dried over magnesium sulfate and the solvent was then distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 750 mg (yield 75%) of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04613613uspto-grants-1986_09