Reaktion #662791

ord-15517f9e59204aadbc7ed7dafba3735d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with dichloromethane (3×10 ml)
  2. 2
    Waschenthe combined organic extracts were washed with saturated bicarbonate solution (aq)
  3. 3
    Trocknendried over sodium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated in vacuo

Vorschrift

Ethylsulfonyl chloride (177 mg, 1.4 mmol) was added dropwise to a stirred solution of 3-bromo-4-(2,4-difluorophenoxy)aniline (328 mg, 1.1 mmol) and pyridine (178 μL, 2.2 mmol) in dichloromethane (2 ml) at 0° C. under nitrogen. After the mixture was allowed to warm to rt and stir overnight, it was treated with 1N HCl (10 ml) and extracted with dichloromethane (3×10 ml); the combined organic extracts were washed with saturated bicarbonate solution (aq), dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound (430 mg, 99%) as a tan solid which was carried forward without purification. LCMS (M−H)−=391.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09034900B2uspto-grants-2015_05