反应 #452461

反应方程式

propane-1,3-diamine

pyridine

→

N-(pyridin-2-yl)propane-1,3-diamine

收率 76.0%

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   温度The reaction mixture was heated
3. 3
   温度at reflux for 18 h
4. 4
   温度cooled
5. 5
   其他the volatiles evaporated in vacuo
6. 6
   workup.ADDITIONTo the residue was added tetrahydrofuran (1 l)
7. 7
   过滤the precipitate was filtered off
8. 8
   洗涤washed with tetrahydrofuran (0.5 l)
9. 9
   其他The solvent was evaporated in vacuo
10. 10
    workup.DISTILLATIONthe residue purified by distillation at 95-97° C.

实验过程

To a solution of propane-1,3-diamine (310 ml, 3.63 mol) in dry pyridine (75 ml) kept under an atmosphere of nitrogen 2-bromopyridine (70 ml, 0.73 mol) was added. The reaction mixture was heated at reflux for 18 h, cooled and the volatiles evaporated in vacuo. To the residue was added tetrahydrofuran (1 l) and the precipitate was filtered off and washed with tetrahydrofuran (0.5 l). The solvent was evaporated in vacuo and the residue purified by distillation at 95-97° C. and 2×10-2 mbar affording 83.37 g (76%) of N-(pyridin-2-yl)propane-1,3-diamine.

来源