반응 #48534

반응 방정식

4-amino-1,2,4-triazole

4-amino-1,2,4-triazole

1-bromopropane

4-amino-1,2,4-triazole acetonitrile

→

1-n-propyl-4-amino-1,2,4-triazolium bromide

수율 97.5%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타equipped with a reflux condenser
2. 2
   기타placed in a hot oil bath
3. 3
   기타(50° C.)
4. 4
   온도to heat
5. 5
   workup.STIRRINGThe reaction mixture was stirred
6. 6
   온도with heating for 36 hours
7. 7
   기타was consumed
8. 8
   기타The flask was then removed from the oil bath
9. 9
   온도cooled under nitrogen atmosphere
10. 10
    기타The reaction solution was transferred to a large round bottomed flask
11. 11
    기타the acetonitrile and excess n-propyl bromide rotary evaporated away
12. 12
    기타The resultant oil was transferred to a preweighed Schlenk flask
13. 13
    세척rinsing the large flask with three 10 ml aliquots of fresh acetonitrile
14. 14
    기타The flask was evacuated for 20 hours

실험 절차

10.005 g 118 mmoles of 4-amino-1,2,4-triazole was weighed out and transferred to a three necked 500 ml, round bottom flask and dissolved 200 ml of acetonitrile. The solution then was stirred vigorously with an overhead stirrer the flask equipped with a reflux condenser and placed in a hot oil bath (50° C.) and allowed to heat. In a graduated cylinder, 1-bromopropane 58.865 g, 478 mmoles, was weighed out and then was slowly added to the hot 4-amino-1,2,4-triazole/acetonitrile mixture. The reaction mixture was stirred with heating for 36 hours, being monitored by thin layer chromatography, at which time the 4-amino-1,2,4-triazole was consumed. The flask was then removed from the oil bath, cooled under nitrogen atmosphere. The reaction solution was transferred to a large round bottomed flask and the acetonitrile and excess n-propyl bromide rotary evaporated away. The resultant oil was transferred to a preweighed Schlenk flask, rinsing the large flask with three 10 ml aliquots of fresh acetonitrile. The flask was evacuated for 20 hours to yield a highly crystalline solid 23.9584 g, 115 mmoles of 1-n-propyl-4-amino-1,2,4-triazolium bromide. Melting point: 63° C.; DSC onset 145° C.,

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