HRID1913217
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
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To a 10-20 mL microwave vessel was charged ethyl 4-((7-chloropyrazolo[1,5-a]pyrimidin-5-yl)methyl)cyclohexanecarboxylate (Int-4g, 2.29 g, 7.12 mmol). To this was added ˜7N NH3 in methanol (15 mL). The resulting solution was stirred at 90° C. for 4 hours. After 4 hours, the reaction was cooled to room temperature and diluted with DCM (100 mL). This solution was washed with H2O and the organic layer was extracted. The aqueous phase was again extracted with DCM. The combined organics were dried over Na2SO4 and then the solvent was removed in vacuo. The resulting solid was taken on without further purification.
WORKUP
后处理
- waitAfter 4 hours
- temperaturethe reaction was cooled to room temperature
- washThis solution was washed with H2O
- extractionthe organic layer was extracted
- extractionThe aqueous phase was again extracted with DCM
- dry with materialThe combined organics were dried over Na2SO4
- customthe solvent was removed in vacuo
- customThe resulting solid was taken on without further purification