Reaktion #576054

ord-0ae6dd2a4d3248d0ac215ee393b83833

Lösungsmittel

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ethyl acetate
  2. 2
    WaschenThe extract was washed with a saturated brine
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    Einengenconcentrated under reduced pressure
  5. 5
    SonstigeThe resultant residue was recrystallized from ethyl acetate-diisopropyl ether

Vorschrift

A solution of 2-(7-chloro-6-hydroxy-2-oxo-4-phenyl-2H-chromen-3-yl)-N-[4-chloro-2-(trifluoromethyl)phenyl]acetamide (Example 208) (0.30 g) in DMF (5 ml) was combined with 2-chloroethyl ethyl ether (0.31 ml), potassium carbonate (0.23 g) and sodium iodide (0.15 g), and stirred at 120° C. for 30 minutes. The reaction solution was combined with water and extracted with ethyl acetate. The extract was washed with a saturated brine, and then dried over magnesium sulfate, and concentrated under reduced pressure. The resultant residue was recrystallized from ethyl acetate-diisopropyl ether to obtain the title compound as a colorless crystal (151 mg, 43%). Melting point: 170-171° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06974806B2uspto-grants-2005_12