反应 #1166457

反应方程式

pyridyl ketone oxime

ammonia

→

Bis(pyridin-2-yl)methylamine

收率 86.0%

溶剂

ethanol

反应条件

后处理

1. 1
   温度The solution was warmed
2. 2
   温度until reflux
3. 3
   温度the mixture was refluxed for 1 h.
4. 4
   过滤The solution was filtered
5. 5
   workup.ADDITIONwater (15 ml) was added
6. 6
   workup.ADDITIONSolid NaOH was added until PH>>10
7. 7
   萃取the solution was extracted with CH2Cl2 (3×20 ml)
8. 8
   干燥The organic layers were dried over Na2SO4
9. 9
   其他evaporated until dryness

实验过程

To pyridyl ketone oxime (3 g, 15.1 mmol) was added ethanol (15 ml), concentrated ammonia solution (15 mL) and NH4OAc (1.21 g, 15.8 mmol). The solution was warmed until reflux. To this solution was added 4.64 g Zn in small portions. After the addition of all Zn, the mixture was refluxed for 1 h. and allowed to cool to ambient temperature. The solution was filtered and water (15 ml) was added. Solid NaOH was added until PH>>10 and the solution was extracted with CH2Cl2 (3×20 ml). The organic layers were dried over Na2SO4 and evaporated until dryness. Bis(pyridin-2-yl)methylamine (2.39 g, 12.9 mmol) was obtained as a colourless oil in 86% yield, showing the following analytical characteristics:

来源