HRID487272
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewere heated
- temperatureunder reflux for 28 hours
- customThe solvent was removed in vacuo
- dissolutionthe residue was dissolved in hot water (25 ml)
- filtrationwas filtered
- filtrationthe resulting white precipitate was collected by filtration
- customrecrystallized from DMF