Reaktion #83230

ord-c651f3fd58b24bc3ba2e2a2a4c9e536d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 3 hours
  2. 2
    Temperaturcooled
  3. 3
    ExtraktionThe separated oil was extracted with dichloromethane
  4. 4
    WaschenThe extract was washed with brine
  5. 5
    Sonstigedried
  6. 6
    Einengenconcentrated in vacuo
  7. 7
    SonstigeThe residue was purified by column chromatography on silica gel
  8. 8
    Sonstigethe obtained oil was crystallized from diisopropyl ether

Vorschrift

A mixture of 8-(4-fluorophenyl)-4-methyl-7-(pyridin-4-yl)pyrazolo[5,1-c][1,2,4]triazine (53 mg) and sodium borohydride (13 mg) in ethanol (1 ml) was refluxed for 3 hours, cooled and poured into ice-water. The separated oil was extracted with dichloromethane. The extract was washed with brine, dried and concentrated in vacuo. The residue was purified by column chromatography on silica gel and the obtained oil was crystallized from diisopropyl ether to give 1,4-dihydro-8-(4-fluorophenyl)-4-methyl-7-(pyridin-4-yl)pyrazolo[5,1-c][1,2,4]triazine (13 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05624931uspto-grants-1997_04