Reaktion #84424

ord-ba52dcdca5224e56bb6328da85a7e25d

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to rt
  2. 2
    Extraktionextracted with CH2Cl2 (50 mL×3)
  3. 3
    TrocknenThe combined organic phases were dried over anhydrous Na2SO4
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigeThe residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1)

Vorschrift

To a solution of 3,4-difluoronitrobenzene (1.59 g, 10 mmol) in DMSO (15 mL) were added K2CO3 (3.04 g, 22 mmol) and di-n-hexylamine (2.04 g, 11 mmol). The mixture was heated at 90° C. overnight, then cooled to rt, diluted with water (50 mL) and extracted with CH2Cl2 (50 mL×3). The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1) to give the title compound as pale yellow oil (2.79 g, 86%).

Quelle

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