Reaktion #46830

ord-b856a0d71a79491b9506c65e836cc788

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenAfter acidification with a 1 M HCL-solution the mixture was concentrated
  2. 2
    SonstigeThe resulting residue was purified by preparative HPLC (CH3CN/H2O gradient+0.05% formic acid)

Vorschrift

20 mg (0.04 mmol) 1-(3-Methoxy-benzyl)-2-[4-(3-oxo-morpholin-4-yl)-phenylcarbamoyl]-1H-benzoimidazole-4-carboxylic acid methyl ester were suspended in 5 mL MeOH. 194 μl (0.19 mmol) of an aqueous 1 M LiOH-solution were added and the resulting mixture was stirred for 8 h at 60° C. After acidification with a 1 M HCL-solution the mixture was concentrated. The resulting residue was purified by preparative HPLC (CH3CN/H2O gradient+0.05% formic acid) to give pure 1-(3-Methoxy-benzyl)-2-[4-(3-oxo-morpholin-4-yl)-phenylcarbamoyl]-1H-benzoimidazole-4-carboxylic acid as a colorless amorphous solid. Yield: 44 mg MS (ES+): m/e=501.

Quelle

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