Reaktion #84538

ord-8556e0a10d2245e59d74de65968a0b5e

Lösungsmittel

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe resulting mixture was extracted with DCM (30 mL×2)
  2. 2
    WaschenThe combined organic phases were washed with brine (30 mL×3)
  3. 3
    Trocknendried over anhydrous Na2SO4
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigeThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=4:1)

Vorschrift

A mixture of 1,2-difluoro-4-nitrobenzene (1.0 g, 6.29 mmol), 2-morpholinoethanol (1.0 g, 7.62 mmol) and Cs2CO3 in DMF (10 mL) was stirred at 75° C. for 12 h. 30 mL of water was then added and the resulting mixture was extracted with DCM (30 mL×2). The combined organic phases were washed with brine (30 mL×3), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=4:1) to give the title compound as yellow oil (1.30 g, 76%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434695B2uspto-grants-2016_09