تفاعل #83232

ord-2bf86c20845747d0b497d8ed708c9cd8

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05624931uspto-grants-1997_04