Reaktion #350757

ord-caee3e87b39c407ca95b6b9f48757ef6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONThe solvent was distilled off
  2. 2
    ExtraktionThe residue was extracted with chloroform
  3. 3
    Waschenwashed
  4. 4
    Sonstigedried
  5. 5
    Sonstigesubjected to solvent removal by distilation
  6. 6
    SonstigeThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol=99/1)
  7. 7
    Sonstigerecrystallized from ethyl acetate

Vorschrift

In 6 ml of chloroform was dissolved 100 mg of 2-(3,4-dimethoxybenzoyl)-4-(3,4-dihydroxycarbostyril-6-yl)thiazole. Thereto was added sodium boron hydride at room temperature, and the mixture was stirred for 1 hour at the same temperature. The solvent was distilled off. The residue was extracted with chloroform. The extract was water-washed, dried and then subjected to solvent removal by distilation. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol=99/1) and then recrystallized from ethyl acetate to obtain 52 mg of 2-[1-(3,4-dimethoxyphenyl)-1-hydroxymethyl]-4-(3,4-dihydroxycarbostyril-6-yl)thiazole as light brown prismatic crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05643932uspto-grants-1997_07