HRID929689

反应详情

EQUATION

反应方程式

HRID 929689 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customcompletion of the reaction
  2. temperatureto cool
  3. customthe solvent was removed in vacuo
  4. customThe resulting crude material was purified by flash chromatography (2% methanol/DCM)