Reaktion #317578

ord-c4b65cd644a1426c80874aaa864a23c7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was quenched with water
  2. 2
    Extraktionextracted with EtOAc
  3. 3
    Trocknendried over Na2SO4
  4. 4
    SonstigeAfter removal of the
  5. 5
    Filtrationdessicant by filtration, concentration
  6. 6
    Sonstigeyielded an orange crude oil
  7. 7
    SonstigeThe crude product was purified by flash chromatography (10%-40% EtOAc/hexanes)

Vorschrift

To 5,6-dichloro-1-methyl-2-isopropenyl-1H-benzimidazole (2.5 g) in acetone (30 mL) and water (6 mL) at room temperature was added trichloroisocyanuric acid (845 mg). The resulting mixture was stirred at room temperature for 18 h. The reaction mixture was quenched with water, extracted with EtOAc, and dried over Na2SO4. After removal of the dessicant by filtration, concentration yielded an orange crude oil. The crude product was purified by flash chromatography (10%-40% EtOAc/hexanes) to yield the title compound as a yellow solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07566733B2uspto-grants-2009_07