Reaktion #83232

ord-2bf86c20845747d0b497d8ed708c9cd8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe resulting clear solution was concentrated in vacuo
  2. 2
    workup.ADDITIONTo the residue was added ethanol (1 ml)
  3. 3
    Einengenthe solution was concentrated in vacuo
  4. 4
    SonstigeThe residue was crystallized from a mixture of methanol (0.5 ml) and ethyl acetate (3 ml)
  5. 5
    Sonstigerecrystallized from an aqueous isopropyl alcohol solution

Vorschrift

To a suspension of 2-(4-fluorophenyl)-3-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine (250 mg) in ethanol (3.5 ml) was added 1N hydrochloric acid (0.85 ml). The resulting clear solution was concentrated in vacuo. To the residue was added ethanol (1 ml) and the solution was concentrated in vacuo. The residue was crystallized from a mixture of methanol (0.5 ml) and ethyl acetate (3 ml) and recrystallized from an aqueous isopropyl alcohol solution to give 2-(4-fluorophenyl)-3-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine hydrochloride (233 mg).

Quelle

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