HRID1426064

反应详情

EQUATION

反应方程式

HRID 1426064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Potassium trimethylsilylamine (5.25 mmol) is added to a solution of (rac.)-1-Aza-bicyclo[3.3.1]nonan-4-ol (5.0 mmol) in THF (20 ml) at room temperature and the solution is stirred for 30 min. The resulting potassium alcoholate is slowly added to a precooled solution of 3,6-dichloropyridazine (7.5 mmol) in THF (50 ml) and the resulting mixture is stirred for another 20 minutes. The solution is allowed to warm to 0° C. is quenched with brine and extracted with diethylether. The organic layer is dried over magnesium sulfate and evaporated. The brown oil is purified by silica gel column chromatography (CH2Cl2:MeOH:NH3, 9:1:0.1) to afford (rac.)-4-(6-Chloro-pyridazin-3-yloxy)-1-aza-bicyclo[3.3.1]nonane (320 mg).

WORKUP

后处理

  1. stirringthe resulting mixture is stirred for another 20 minutes
  2. customis quenched with brine
  3. extractionextracted with diethylether
  4. dry with materialThe organic layer is dried over magnesium sulfate
  5. customevaporated
  6. customThe brown oil is purified by silica gel column chromatography (CH2Cl2:MeOH:NH3, 9:1:0.1)