反应详情

温度

80 °C

In a 40 mL scintillation vial was combined 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine (Int-5g, 5.54 mmol, 1.52 g), EtOH (10 mL), H2O (4 mL) and 4N HCl:dioxane (4 mL). The vial was capped, sealed and the reaction was heated to 80° C. overnight. After 18 hours, the reaction was cooled to room temperature and diluted with DCM (100 mL). The solution was washed with saturated NaHCO3(aq) and extracted with DCM twice more. The combined organics were dried over Na2SO4 and the solvent was removed in vacuo to yield 4-(7-aminopyrazolo[1,5-a]pyrimidin-5-yl)cyclohexanone (Int-5h) (1.18 g, 93% yield) as a pale orange solid.

1. customThe vial was capped
2. customsealed
3. temperaturethe reaction was cooled to room temperature
4. washThe solution was washed with saturated NaHCO3(aq)
5. extractionextracted with DCM twice more
6. dry with materialThe combined organics were dried over Na2SO4
7. customthe solvent was removed in vacuo