HRID431996

反应详情

EQUATION

反应方程式

HRID 431996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-cyanopyridine (0.18 mL, 1.86 mmol) in methanol (5 mL) was treated with sodium metal (12.8 mg, 0.56 mmol) a stirred at ambient temperature for 1 hour. The reaction mixture was then treated with a solution of 3-cyanobenzhyrazide (0.30 g, 1.86 mmol) in methanol (5 mL) and heated at reflux for 3 hours. The reaction mixture was then concentrated in vacuo. The resulting yellow solid was dissolved in toluene (2 mL) and heated overnight at 175° C. The reaction mixture was concentrated in vacuo. Silica gel chromatography using 2% methanol in dichloromethane afforded 0.12 g (26%) of 2-(2-pyridyl)-5-(3-cyanophenyl)-1,3,4-triazole.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 3 hours
  3. concentrationThe reaction mixture was then concentrated in vacuo
  4. dissolutionThe resulting yellow solid was dissolved in toluene (2 mL)
  5. temperatureheated overnight at 175° C
  6. concentrationThe reaction mixture was concentrated in vacuo