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
- 100 °C
PROCEDURE
实验过程
N-(3-(6-chloro-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yl)phenyl)acrylamide (50 mg, 0.130 mmol), 5-amino-2-morpholinophenol (25.3 mg, 0.130 mmol) and potassium carbonate (45.0 mg, 0.326 mmol) were dissolved in t-BuOH (80 mL). 4,5-Bis(diphenylphosphino)-9,9-dimethylxanthene (3.01 mg, 5.21 μmol) and Pd2dba3 (2.386 mg, 2.61 μmol) were then added to the solution. The reaction mixture was refluxed at 100° C. for 12 h, and the reaction was monitored by TLC. Following completion of the reaction, the reaction mixture was allowed to cool, and the solvent was removed in vacuo. The resulting crude material was purified by flash chromatography (2% methanol/DCM) to yield the title compound (20 mg, 0.037 mmol, 28.3% yield) as yellow solid. Crude material was used without further purification and used directly in the next reaction.
WORKUP
后处理
- customcompletion of the reaction
- temperatureto cool
- customthe solvent was removed in vacuo
- customThe resulting crude material was purified by flash chromatography (2% methanol/DCM)