Reaktion #736402

ord-c0528f99b79745eb8301ef22c90254af

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added dropwise under ice-
  2. 2
    Temperaturcooling over 5 minutes
  3. 3
    WaschenThe reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate
  4. 4
    Trocknena saturated saline, and dried with anhydrous magnesium sulfate
  5. 5
    SonstigeThe solvent was evaporated
  6. 6
    Sonstigethe residue was purified by column chromatography

Vorschrift

5-Methoxy-2-[[3-methoxy-4-(2,2,2-trifluoroethoxy)pyrid-2-yl]methylthio]benzimidazole (989 mg) was dissolved in chloroform (30 ml), to which a solution of m-chloroperbenzoic acid (503 mg) in chloroform (8 ml) was added dropwise under ice-cooling over 5 minutes. The reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and then a saturated saline, and dried with anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified by column chromatography, to give 5-methoxy-2-[[3-methoxy-4-(2,2,2-trifluoroethoxy)pyrid-2-yl)methylsulfinyl]benzimidazole (712 mg) as a light brownish yellow powder. m.p. 36°-46° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04738975uspto-grants-1988_04