Reaktion #170251

ord-8de270e2961e40b584112b0213076379

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was then heated up
  2. 2
    Temperaturto reflux
  3. 3
    SonstigeThe aqueous phase was separated
  4. 4
    Extraktionextracted with ethyl acetate (2×70 mL)
  5. 5
    WaschenThe combined organic phases were washed with a saturated solution of sodium chloride (40 mL)
  6. 6
    Trocknendried over sodium sulfate
  7. 7
    Filtrationfiltered
  8. 8
    Einengenconcentrated to dryness

Vorschrift

Potassium iodide (530 mg, 3.14 mmol) was added to a solution of 1-benzhydrylazetidin-3-yl methanesulfonate (500 mg, 1.57 mmol) in a mixture of water (2.5 mL) and 1,2-dimethoxyethane (2.5 mL) at room temperature. The reaction mixture was then heated up to reflux and stirred for 3 hours. After cooling down to room temperature, the reaction mixture was diluted by addition of water (50 mL) and ethyl acetate (50 mL). The aqueous phase was separated and extracted with ethyl acetate (2×70 mL). The combined organic phases were washed with a saturated solution of sodium chloride (40 mL), dried over sodium sulfate, filtered and concentrated to dryness. The title compound was obtained as a yellow solid (550 mg, 100%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846711B2uspto-grants-2014_09