Reaktion #348159

ord-748b7a01d7264ac9a314cd52615b7bd7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction was refluxed for 12 hours
  2. 2
    SonstigeThe solid was removed by vacuum filtration through celite
  3. 3
    Waschenwas washed with ethyl acetate
  4. 4
    WaschenThe filtrate was washed with 10% NaHCO3
  5. 5
    Trocknendried over MgSO4

Vorschrift

Trans-2-(4-allyloxy-3-methoxy-5-nitrophenyl)-4-(3,4,5-trimethoxy-phenyl)-1,3-dithiolane (24) 2.60 g, 5.43 mmole) was predissolved in 33 ml absolute ethanol. To this solution was added calcium chloride (0.602 g, 5.43 mmole) predissolved in 7 ml H2O followed by freshly activated zinc dust (7.09 g, 108 mmole). The reaction was refluxed for 12 hours. The solid was removed by vacuum filtration through celite and was washed with ethyl acetate. The filtrate was washed with 10% NaHCO3, dried over MgSO4, and

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05530141uspto-grants-1996_06