HRID596416

反应详情

EQUATION

反应方程式

HRID 596416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
245 °C

PROCEDURE

实验过程

To 4-cyanopyridine (4.2 g.) in methanol (60 ml.) is added sodium (0.2 g.). The solution is allowed to stand for 0.5 hour at room temperature and is then added to a suspension of p-aminobenzhydrazide (6.4 g.) in 150 ml. of methanol. The resulting solution is heated 20 hours at reflux during which time a solid separates. The solid is filtered and heated to 245° C. over 1 hour and maintained at that temperature for an additional 15 minutes. After cooling the solid is recrystallized from a mixture of acetonitrile and water to yield 3-(p-aminophenyl)-5-(4-pyridyl)-1,2,4-triazole (2 g.) m.p. 251°-252.5° C.

WORKUP

后处理

  1. temperatureThe resulting solution is heated 20 hours
  2. temperatureat reflux during which time a solid separates
  3. filtrationThe solid is filtered
  4. temperaturemaintained at that temperature for an additional 15 minutes
  5. temperatureAfter cooling the solid
  6. customis recrystallized from a mixture of acetonitrile and water