반응 #48535

반응 방정식

4-amino-1,2,4-triazole

Ethyl bromide

4-amino-1,2,4-triazole

→

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

용매

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   기타A 500 ml round bottom flask equipped with an overhead stirrer
2. 2
   기타had been consumed
3. 3
   기타The resultant solution was then rotary evaporated down
4. 4
   기타to leave a colorless oil which
5. 5
   기타slowly crystallized
6. 6
   온도Solid material was heated to 60 C
7. 7
   workup.WAITfor 5 hours under high vacuum
8. 8
   기타Crystalline 1-ethyl-4-amino-1,2,4-triazolium bromide was recovered in essentially quantitative yield and high purity, 22.94 g, 117 mmoles
9. 9
   기타150° C.

실험 절차

A 500 ml round bottom flask equipped with an overhead stirrer was charged with 10.00 grams of 4-amino-1,2,4-triazole and 200 ml of acetonitrile. Ethyl bromide, 45 ml, 65.0 grams, was added to the vigorously stirred acetonitrile reaction mixture. The reaction was stirred for 8 days at ambient temperature at which time, thin layer chromatography showed that all of the 4-amino-1,2,4-triazole had been consumed. The resultant solution was then rotary evaporated down to leave a colorless oil which slowly crystallized. Solid material was heated to 60 C. for 5 hours under high vacuum, whereupon it melted and lost the remaining solvent and resolidified. Crystalline 1-ethyl-4-amino-1,2,4-triazolium bromide was recovered in essentially quantitative yield and high purity, 22.94 g, 117 mmoles. Melting point: 63-67° C.; DSC onset: 150° C.

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