Reaktion #160631

ord-2ee651f412704a40bed080bb95e0af14

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water (2×), brine
  2. 2
    Trocknendried over Na2SO4
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigepurified by flash chromatography on a silica gel column (hex:ethyl acetate 4:1)

Vorschrift

To a stirred solution of Ethyl 2-(3-hydroxyphenyl)acetate (4 g, 22.2 mmol) in DMF (20 ml) was added potassium carbonate (4 g, 28.9 mmol) at room temperature followed by drop wise addition of 2,6-Difluorobenzyl bromide (5.06 g, 24.4 mmol). The reaction mixture was stirred for 12 hours and taken in ethyl acetate, washed with water (2×), brine, dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (hex:ethyl acetate 4:1) to give the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829058B2uspto-grants-2014_09