HRID1180686

反应详情

EQUATION

反应方程式

HRID 1180686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

To a flask was added a mixture of 6 g [1,10]phenanthroline-2-carbonitrile, 3.1 g NH4Cl, 3.8 g NaN3, 0.01 g LiCl and 60 ml DMF, and the mixture was then heated to 120-130° C. and stirred overnight. After completion of reaction, the reaction mixture was cooled to room temperature, filtered to remove solids, and vacuum distallated to remove DMF, and then 300 ml water was added. Next, HCl(aq) was added to adjust pH value to about 4, and stirred for 30 minutes. Finally, the solution was filtered to give solids, and then the solids were washed by water and dried to obtain products 2-(1H-tetrazol-5-yl)-[1,10]phenanthroline 6.1 g. (yield=84.0%).

WORKUP

后处理

  1. additionTo a flask was added
  2. customAfter completion of reaction
  3. temperaturethe reaction mixture was cooled to room temperature
  4. filtrationfiltered
  5. customto remove solids, and vacuum
  6. customto remove DMF
  7. addition300 ml water was added
  8. additionNext, HCl(aq) was added
  9. stirringstirred for 30 minutes
  10. filtrationFinally, the solution was filtered
  11. customto give solids
  12. washthe solids were washed by water
  13. customdried