Reaktion #302941

ord-8f4c30c8705148e7a0a39fc309356f2a

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was cooled to room temperature
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    WaschenThe organic layer was washed with water and brine
  4. 4
    Trocknendried over sodium sulfate
  5. 5
    Einengenconcentrated under reduced pressure
  6. 6
    SonstigeThe resulting residue was purified by silica gel column chromatography (eluting solvent: n-hexane:ethyl acetate=10:1)

Vorschrift

A suspension of 1-(3-chloropropoxy)-4-iodobenzene obtained in Example 1-(1) (2.79 g), (R)-2-methylpyrrolidine (0.961 g), sodium iodide (0.282 g) and potassium carbonate (2.60 g) in acetonitrile (2.8 mL) was stirred in a sealed tube at 100° C. for 5 hours. The reaction mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluting solvent: n-hexane:ethyl acetate=10:1) to give the titled compound (3.27 g) as a yellow oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08193176B2uspto-grants-2012_06