Reaktion #5086

ord-15280f38c7e244d1bfa07303e59094ac

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe reaction mixture was extracted with 100 ml of ethyl acetate
  2. 2
    Waschenthe extract was washed 5 times with 100 ml of water
  3. 3
    Trocknendried with anhydrous magnesium sulfate
  4. 4
    SonstigeThe solvent was removed by evaporation
  5. 5
    Sonstigeto obtain the residue which
  6. 6
    Sonstigewas purified by means of a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1)

Vorschrift

To a mixture of 1.50 g of 4-(3-chlorophenyl)-piperazine and 0.31 g of sodium hydride was added 2.4 ml of epichlorohydrin and the reaction mixture as stirred at room temperature for 30 minutes. After the reaction was completed, the reaction mixture was extracted with 100 ml of ethyl acetate, and the extract was washed 5 times with 100 ml of water, then dried with anhydrous magnesium sulfate. The solvent was removed by evaporation to obtain the residue which was purified by means of a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1) to obtain 1.66 g of 4-(3-chlorophenyl)-1-(2,3-epoxypropyl)piperazine as in the form of an oily substance.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05242919uspto-grants-1993_09