반응 #48533

반응 방정식

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

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타had been consumed
3. 3
   온도to cool to room temperature
4. 4
   기타was rotary evaporated down
5. 5
   기타to leave a viscous oil
6. 6
   workup.DISSOLUTIONdissolving it

실험 절차

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.

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