HRID1931605

反应详情

EQUATION

反应方程式

HRID 1931605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

4-(Methylsulfonyl)-phenol (Oakwood Products, Inc., West Columbia, S.C., USA; 516 mg, 3 mmol) and cesium carbonate (1.63 g, 5 mmol) were added to a solution of 4-chloro-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidine (from Step 1; 610 mg, 2.56 mmol) in dimethylformamide (15 mL). The mixture was heated at 90° C. for 1 h, then cooled, poured into saturated aqueous sodium bicarbonate solution, and extracted three times with ethyl acetate. The combined organic extracts were washed with twice with water and once with brine, dried (magnesium sulfate), filtered, and evaporated to give 4-(4-methanesulfonyl-phenoxy)-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidine (780 mg, 58%).

WORKUP

后处理

  1. temperaturecooled
  2. extractionextracted three times with ethyl acetate
  3. washThe combined organic extracts were washed with twice with water
  4. dry with materialonce with brine, dried (magnesium sulfate)
  5. filtrationfiltered
  6. customevaporated