반응 #83232

ord-2bf86c20845747d0b497d8ed708c9cd8

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05624931uspto-grants-1997_04