تفاعل #1166457

معادلة التفاعل

pyridyl ketone oxime

ammonia

→

Bis(pyridin-2-yl)methylamine

المردود 86.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution was warmed
2. 2
   درجة الحرارةuntil reflux
3. 3
   درجة الحرارةthe mixture was refluxed for 1 h.
4. 4
   ترشيحThe solution was filtered
5. 5
   workup.ADDITIONwater (15 ml) was added
6. 6
   workup.ADDITIONSolid NaOH was added until PH>>10
7. 7
   استخلاصthe solution was extracted with CH2Cl2 (3×20 ml)
8. 8
   تجفيفThe organic layers were dried over Na2SO4
9. 9
   أخرىevaporated until dryness

الإجراء التجريبي

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:

المصدر