Reaktion #425419

ord-fccc59a3df954415be06fc4bd4e20550

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated in vacuo
  2. 2
    Sonstigeto give a yellow oil
  3. 3
    Waschenwashed with 1N HCl and saturated NaHCO3
  4. 4
    Trocknendried over sodium sulfate
  5. 5
    Einengenconcentrated in vacuo

Vorschrift

To a solution of 3-(4-bromophenoxy)azetidine (207 mg, 0.91 mmol) in CH2Cl2 (10 mL) was added triethylamine (276 mg, 2.73 mmol) and acetic anhydride (186 mg, 1.82 mmol). The mixture was stirred at room temperature overnight. The reaction mixture was concentrated in vacuo to give a yellow oil. The crude product was diluted with ethyl acetate (20 mL), washed with 1N HCl and saturated NaHCO3, dried over sodium sulfate, and concentrated in vacuo to give 1-[3-(4-bromophenoxy)azetidin-1-yl]ethanone (245 mg, 100%) as a colorless oil. 1H NMR (400 MHz, CDCl3) δ 7.40 (d, 2H), 6.61 (d, 2H), 4.89 (m, 1H), 4.49 (m, 1H), 4.37 (m, 1H), 4.17 (m, 1H), 4.03 (m, 1H), 1.90 (s, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08889730B2uspto-grants-2014_11