반응 #1166457

반응 방정식

pyridyl ketone oxime

ammonia

→

Bis(pyridin-2-yl)methylamine

수율 86.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도The solution was warmed
2. 2
   온도until reflux
3. 3
   온도the mixture was refluxed for 1 h.
4. 4
   여과The solution was filtered
5. 5
   workup.ADDITIONwater (15 ml) was added
6. 6
   workup.ADDITIONSolid NaOH was added until PH>>10
7. 7
   추출the solution was extracted with CH2Cl2 (3×20 ml)
8. 8
   건조The organic layers were dried over Na2SO4
9. 9
   기타evaporated until dryness

실험 절차

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:

출처