反应 #452481

反应方程式

1-Formyl-4-(2-quinolylmethyl)piperazine

sulfuric acid

→

title compound

收率 97.6%

1-(2-quinolylmethyl)piperazine

收率 97.6%

溶剂

ethanol

反应条件

后处理

1. 1
   温度After the resulting mixture was heated
2. 2
   温度under reflux
3. 3
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
4. 4
   workup.DISSOLUTIONThe thus-obtained residue was dissolved in water
5. 5
   洗涤After the resulting solution was washed twice with chloroform
6. 6
   萃取followed by extraction with chloroform
7. 7
   洗涤The extract was washed with water
8. 8
   干燥dried over anhydrous magnesium sulfate
9. 9
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

实验过程

1-Formyl-4-(2-quinolylmethyl)piperazine (86.00 g, 332 mmol) was dissolved in ethanol (800 ml), followed by the addition of concentrated sulfuric acid (49.04 g, 500 mmol). After the resulting mixture was heated under reflux and stirring for 4 days, the solvent was distilled off under reduced pressure. The thus-obtained residue was dissolved in water. After the resulting solution was washed twice with chloroform, the solution was rendered basic with a 10N aqueous solution of sodium hydroxide, followed by extraction with chloroform. The extract was washed with water and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, whereby 73.65 g of the title compound were obtained as a pale amber oil (yield: 97.6%).

来源