HRID80904

反应详情

EQUATION

反应方程式

HRID 80904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 4-[6-(4-isopropylpiperazin-1-yl)pyridazin-3-yl]benzonitrile (0.36 g, 1.17 mmol, prepared by a similar procedure to that described in Example 1) in dry THF (5 mL) was added a 1.4 M methylmagnesium bromide solution in toluene/THF. The reaction mixture was stirred at room temperature for 24 h, 1 M hydrochloric acid (7 mL) was added and the solution stirred for 1 h. The mixture was made alkaline by addition of excess NaHCO3 solution and extracted with dichloromethane. The organic phase was dried over magnesium sulphate, the solvent was removed and the solid was re-crystallized from ethanol to give the title compound, 163 mg (43%).

WORKUP

后处理

  1. customprepared by a similar procedure to
  2. stirringthe solution stirred for 1 h
  3. extractionextracted with dichloromethane
  4. dry with materialThe organic phase was dried over magnesium sulphate
  5. customthe solvent was removed
  6. customthe solid was re-crystallized from ethanol