Reaktion #7513

ord-1b563b66a76d47b3b1470b157246b957

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONThe obtained residue was dissolved in ethyl acetate
  3. 3
    Waschenwashed with saturated aqueous sodium hydrogencarbonate solution (×3) and saturated brine (×1)
  4. 4
    Trocknendried over anhydrous sodium sulfate
  5. 5
    EinengenThe solvent was concentrated under reduced pressure

Vorschrift

To ethyl 4-hydroxy-2-(2,3-dihydro-1H-indol-1-yl)-5-pyrimidinecarboxylate (2.85 g, 10 mmol) was added phosphorus oxychloride (10 mL, 2 mmol) and the mixture was stirred at 120° C. for 15 h. The reaction mixture was concentrated under reduced pressure. The obtained residue was dissolved in ethyl acetate, washed with saturated aqueous sodium hydrogencarbonate solution (×3) and saturated brine (×1) and dried over anhydrous sodium sulfate. The solvent was concentrated under reduced pressure to give the title compound (2.9 g, 100%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087597B1uspto-grants-2006_08