Reaktion #214885

Reaktionsgleichung

Sodium

2-cyanopyrazine

pyrazine carboxylic acid hydrazide

→

3,5-DIPYRAZINYL-1,2,4-TRIAZOLE

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture is heated
2. 2
   Temperaturat reflux for 2 hours
3. 3
   workup.WAITat room temperature for 16 hours
4. 4
   TemperaturAfter cooling
5. 5
   Sonstigethe intermediate acylamidrazone is removed by filtration
6. 6
   Temperaturis then heated at temperatures between 200° to 260° C. over two and one-half hours
7. 7
   TemperaturAfter cooling
8. 8
   Sonstigerecrystallization from methanol-water, 0.8 grams of 3,5-dipyrazinyl-1,2,4-triazole
9. 9
   Sonstigem.p. 269°-270.5° C. is obtained

Vorschrift

Sodium (50 mg.) is added to 2-cyanopyrazine (1 gram, 0.01 mole) in 20 ml. of methanol. The solution is allowed to stand 1 hour at room temperature and is added to a suspension of pyrazine carboxylic acid hydrazide (1.4 grams, 0.1 mole) in 50 ml. of methanol. The reaction mixture is heated at reflux for 2 hours and then at room temperature for 16 hours. After cooling, the intermediate acylamidrazone is removed by filtration and is then heated at temperatures between 200° to 260° C. over two and one-half hours. After cooling and recrystallization from methanol-water, 0.8 grams of 3,5-dipyrazinyl-1,2,4-triazole, m.p. 269°-270.5° C. is obtained.

Quelle