反应详情

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.,

1. customequipped with a reflux condenser
2. customplaced in a hot oil bath
3. custom(50° C.)
4. temperatureto heat
5. stirringThe reaction mixture was stirred
6. temperaturewith heating for 36 hours
7. customwas consumed
8. customThe flask was then removed from the oil bath
9. temperaturecooled under nitrogen atmosphere
10. customThe reaction solution was transferred to a large round bottomed flask
11. customthe acetonitrile and excess n-propyl bromide rotary evaporated away
12. customThe resultant oil was transferred to a preweighed Schlenk flask
13. washrinsing the large flask with three 10 ml aliquots of fresh acetonitrile
14. customThe flask was evacuated for 20 hours