反应详情

5-Methyl-pyrazolo[1,5-a]pyrimidin-7-ol/7-Methyl-imidazo[1,2-a]pyrimidin-5-ol/5-Methyl-[1,2,4]triazolo[1,5-a]-pyrimidin-7-ol (3c) (6.5 mmol) was added to 1.82 ml (19.5 mmol) of phosphorus oxychloride and heated under reflux for 30-60 minutes. in a round bottom flask, during which time the solid dissolved and hydrogen chloride was evolved. Excess phosphorus oxychloride was removed by distillation at reduced pressure on a steam-bath and the residue triturated with ice water. Product was extracted from the aqueous mixture with methylene chloride, evaporated and purified by column chromatography using 60% EtOAc/Hexane at a yield of 42-70%.

1. temperatureheated
2. temperatureunder reflux for 30-60 minutes
3. dissolutionin a round bottom flask, during which time the solid dissolved
4. customExcess phosphorus oxychloride was removed by distillation at reduced pressure on a steam-bath
5. customthe residue triturated with ice water
6. extractionProduct was extracted from the aqueous mixture with methylene chloride
7. customevaporated
8. custompurified by column chromatography