Reaktion #2259219

ord-2054d7a1c1aa4ecc9207d1f1402d14fa

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was then partitioned between dichloromethane (20 mL)
  2. 2
    SonstigeThe aqueous layer was separated
  3. 3
    Extraktionextracted with dichloromethane (2×10 mL)
  4. 4
    TrocknenThe combined organic phases were dried over sodium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated to dryness
  7. 7
    SonstigeThe residue was purified by chromatography on silica gel

Vorschrift

A solution of 1-benzhydrylazetidin-3-yl methanesulfonate (324 mg, 1.0 mmol) in thiophene ethanol (2.3 mL, 20.4 mmol) was stirred under microwave irradiations (100 W) at 110° C. for 30 minutes. The reaction mixture was then partitioned between dichloromethane (20 mL) and a solution of sodium hydroxyde (1N, 10 mL). The aqueous layer was separated and extracted with dichloromethane (2×10 mL). The combined organic phases were dried over sodium sulfate, filtered and concentrated to dryness. The residue was purified by chromatography on silica gel, using petroleum ether/ethyl acetate (85:15) as eluent. The title product was obtained as a yellow solid (210 mg, 59%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09051321B2uspto-grants-2015_06