Reaktion #821722

ord-32726f93c4c14104ab85f32f9cb665a8

Lösungsmittel

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was cooled to room temperature
  2. 2
    Einengenconcentrated to 2 vol
  3. 3
    workup.ADDITIONdiluted with ethyl acetate (7 vol)
  4. 4
    WaschenThe organic layer was washed with saturated aqueous ammonium chloride solution (2×3 vol)
  5. 5
    SonstigeThe organic layer was evaporated to dryness

Vorschrift

2-[3-(2-Oxo-1-imidazolidinyl)phenyl]ethyl methanesulfonate (1.32 wt) and 2-methyl-5-(1-piperazinyl)quinoline (1 wt.) were suspended in acetonitrile (5 vol) at room temperature under nitrogen. Diisopropylethylamine (1.53 vol) was added dropwise over 30 minutes, and the mixture was then stirred at 75° C. for 4 hours. The reaction mixture was cooled to room temperature, concentrated to 2 vol, and diluted with ethyl acetate (7 vol). The organic layer was washed with saturated aqueous ammonium chloride solution (2×3 vol), followed by water (1×3 vol). The organic layer was evaporated to dryness, yielding the title compound as a brown foam (70% th).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07592346B2uspto-grants-2009_09