HRID329609

反应详情

EQUATION

反应方程式

HRID 329609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a solution of 22 g of N'-formylnicotinic acid hydrazide in 150 ml of pyridine are added, in portions, 28 g of phosphorus pentasulfide. During this addition the temperature rises to 65° C. After 5 minutes the mixture is heated to 110° C. and stirred for 2 hours at this temperature. The pyridine is then distilled off in a water jet vacuum. The residue is taken up in chloroform and the solution is extracted with a 5% sodium hydroxide solution and water. The organic phase is dried and the solvent is removed by evaporation, affording 2-(3-pyridyl)-1,3,4-thiadiazole as a pale yellow powder with a melting point of 78°-79° C.

WORKUP

后处理

  1. additionDuring this addition the temperature
  2. customrises to 65° C
  3. distillationThe pyridine is then distilled off in a water jet vacuum
  4. extractionthe solution is extracted with a 5% sodium hydroxide solution and water
  5. customThe organic phase is dried
  6. customthe solvent is removed by evaporation