HRID487272

反应详情

EQUATION

反应方程式

HRID 487272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(2-hydroxycyclopentyl)-3-methyl-1H-pyrazole-4-carboxamide (2.4 g, 10 mmol), 4-pyridinecarboxamidine hydrochloride (3.2 g, 20 mmol), potassium carbonate (2.8 g, 20 mmol) and DMF (50 ml) were heated under reflux for 28 hours. The solvent was removed in vacuo, the residue was dissolved in hot water (25 ml) and was filtered. The filtrate was acidified with acetic acid and the resulting white precipitate was collected by filtration and recrystallized from DMF to afford 0.73 g (21%) of 1-(2-hydroxycyclopentyl)-3-methyl-6-(4-pyridyl)-pyrazolo[3,4-d]pyrimidin-4-one as white needles, m.p. 281°-283° C.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureunder reflux for 28 hours
  3. customThe solvent was removed in vacuo
  4. dissolutionthe residue was dissolved in hot water (25 ml)
  5. filtrationwas filtered
  6. filtrationthe resulting white precipitate was collected by filtration
  7. customrecrystallized from DMF