反応 #1166457

反応方程式

pyridyl ketone oxime

ammonia

→

Bis(pyridin-2-yl)methylamine

収率 86.0%

溶媒

ethanol

反応条件

後処理

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
   ろ過The solution was filtered
5. 5
   workup.ADDITIONwater (15 ml) was added
6. 6
   workup.ADDITIONSolid NaOH was added until PH>>10
7. 7
   抽出the solution was extracted with CH2Cl2 (3×20 ml)
8. 8
   乾燥The organic layers were dried over Na2SO4
9. 9
   その他evaporated until dryness

実験手順

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:

出典