反应 #48533

反应方程式

4-amino-1,2,4-triazole

isopropyl alcohol

4-amino-1,2,4-triazole

2-bromoethanol

→

1-ethanol 4-amino-1,2,4-triazolium bromide

溶剂

acetonitrile

反应条件

后处理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   其他had been consumed
3. 3
   温度to cool to room temperature
4. 4
   其他was rotary evaporated down
5. 5
   其他to leave a viscous oil
6. 6
   workup.DISSOLUTIONdissolving it

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.

来源