Reaktion #46811

ord-ce1eae390e274e7aaf0ec5c11672db47

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with 40 mL of a saturated NaHCO3-solution
  2. 2
    ExtraktionThe aqueous solution was extracted with CH2Cl2 (3×200 ml)
  3. 3
    Trocknenthe combined organic layers were dried over MgSO4
  4. 4
    Einengenconcentrated under reduced pressure
  5. 5
    Sonstigeto give a brown solid, which

Vorschrift

A solution of 769 mg 2-Trichloromethyl-1H-benzoimidazole in 10 mL THF were slowly added to a mixture containing 304 mg 1-(4-Amino-phenyl)-1H-pyridin-4-one, 1.3 g NaHCO3, 40 mL THF and 15 mL H2O. The mixture was stirred vigorously for 3 h at room temperature, diluted with 200 mL CH2Cl2 and washed with 40 mL of a saturated NaHCO3-solution. The aqueous solution was extracted with CH2Cl2 (3×200 ml) and the combined organic layers were dried over MgSO4 and concentrated under reduced pressure to give a brown solid, which was pure enough for the following reactions.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741341B2uspto-grants-2010_06