Reaktion #362900

ord-9e3f61f2e9b143809cf4cccbc7248b97

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 3 h
  2. 2
    Filtrationfiltered
  3. 3
    Einengenconcentrated in vacuo
  4. 4
    SonstigeThe residue was purified on silica gel
  5. 5
    Wascheneluted with ethyl acetate-heptane (1:2)
  6. 6
    Sonstigeto give a crystalline compound, which
  7. 7
    Sonstigewas recrystallized (ethyl acetate)

Vorschrift

A mixture of 4-(piperazin-1-yl)-1H-indole (1.5 g), 2-(2-iodoethyl)indane (2.0 g), K2CO3, methyl isobutyl ketone (150 ml), and N-methylpyrrolidone (10 ml) was boiled under reflux for 3 h. The mixture was allowed to cool to room temperature, filtered, and concentrated in vacuo. The residue was purified on silica gel eluted with ethyl acetate-heptane (1:2) to give a crystalline compound, which was recrystallized (ethyl acetate) to give the title compound (1.2 g, 47%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06352988B2uspto-grants-2002_03