Реакция #83224

ord-dd01f07c44a84993bf43d21351f9b531

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas refluxed for 8 hours
  2. 2
    ТемператураThe mixture was cooled
  3. 3
    Концентрированиеconcentrated in vacuo
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in a mixture of acetic acid (10 ml) and concentrated hydrochloric acid (1.5 ml)
  5. 5
    ТемператураThe solution was refluxed for 2 hours
  6. 6
    Температураcooled
  7. 7
    ДругоеThe separated solid was collected
  8. 8
    Промывкаwashed with water
  9. 9
    Другоеdried

Методика

A mixture of 5-amino-3-(4-fluorophenyl)-4-(pyridin-4-yl)pyrazole (1.016 g), methyl acrylate (10 ml), pyridine (20 ml) and water (5 ml) was refluxed for 8 hours. The mixture was cooled and concentrated in vacuo. The residue was dissolved in a mixture of acetic acid (10 ml) and concentrated hydrochloric acid (1.5 ml). The solution was refluxed for 2 hours, cooled and neutralized with an aqueous saturated sodium bicarbonate solution. The separated solid was collected, washed with water and dried to give 2-(4-fluorophenyl)-5-oxo-3-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine (750 mg).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05624931uspto-grants-1997_04