HRID20255

反应详情

EQUATION

反应方程式

HRID 20255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

5.000 grams, 59.4 mmoles of 4-amino-1,2,4-triazole was dissolved in 200 ml of fresh acetonitrile and stirred vigorously. 29.800 grams of 2-bromoethanol was added slowly to the solution by pipet. After the addition was complete, the reaction mixture was heated for 20 hours at 80° C., until thin layer chromatography revealed that all of the 4-amino-1,2,4-triazole had been consumed. The reaction mixture was then allowed to cool to room temperature and then was rotary evaporated down to leave a viscous oil. Hot isopropyl alcohol was added to the oil dissolving it. Storage of the resultant solution in a refrigerator resulting in a large crop of a viscous oil of 1-ethanol-4-amino-1,2,4-triazolium bromide, 9.9332 g, 47.5 mmoles. Melting point 0-5° C.; DSC onset 180° C.

WORKUP

后处理

  1. additionAfter the addition
  2. customhad been consumed
  3. temperatureto cool to room temperature
  4. customwas rotary evaporated down
  5. customto leave a viscous oil
  6. dissolutiondissolving it