HRID1396808

反应详情

EQUATION

反应方程式

HRID 1396808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 4-(5-amino-2-(pyridin-3-yl)thiazolo[5,4-d]pyrimidin-7-yl)-N-p-tolylpiperazine-1-carboxamide (90 mg, 0.2 mmol) in DMF (5 ml) was added NaH (60%, 12 mg, 0.31 mmol). The resulting mixture was stirred at room temperature for 10 minutes. Then, methyl iodide (0.3 mmol) was added to the mixture. After stirring at room temperature for 30 minutes, the solvents were evaporated in vacuo and the crude residue was purified by flash chromatography on silica, the mobile phase being a mixture of methanol and dichloromethane (in a ratio of 1/30), yielding the pure title compound as yellowish solid (40 mg, 43%).

WORKUP

后处理

  1. stirringAfter stirring at room temperature for 30 minutes
  2. customthe solvents were evaporated in vacuo
  3. customthe crude residue was purified by flash chromatography on silica
  4. additiona mixture of methanol and dichloromethane (in a ratio of 1/30),