Reaktion #985766

ord-b0f172d4b6874120b10e0f4653046180

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenphase was washed with water, saturated aqueous sodium bicarbonate and saturated aqueous NaCl
  2. 2
    Trocknendried over magnesium sulphate
  3. 3
    Sonstigeevaporated down i
  4. 4
    SonstigeColumn chromatography (silica gel, gradient dichloromethane/MeOH 100:0→19:1) yielded the product

Vorschrift

A solution of 2.650 g (11.000 mmol) 2-bromo-4-trifluoromethyl-phenol and 1.47 mL 13.20 mmol) ethyl bromo-acetate in 20 mL Hünig base was stirred for 5 h at 120° C. The reaction mixture was diluted with EtOAc and the org. phase was washed with water, saturated aqueous sodium bicarbonate and saturated aqueous NaCl, dried over magnesium sulphate and evaporated down i. vac. Column chromatography (silica gel, gradient dichloromethane/MeOH 100:0→19:1) yielded the product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07351719B2uspto-grants-2008_04