HRID263123

反应详情

EQUATION

反应方程式

HRID 263123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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, 0.01 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.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for 2 hours
  3. waitat room temperature for 16 hours
  4. temperatureAfter cooling
  5. customthe intermediate acylamidrazone is removed by filtration
  6. temperatureis then heated at temperatures between 200° to 260° C. over two and one-half hours
  7. temperatureAfter cooling
  8. customrecrystallization from methanol-water, 0.8 grams of 3,5-dipyrazinyl-1,2,4-triazole
  9. customm.p. 269°-270.5° C. is obtained