반응 #48538

반응 방정식

diethyl ether

4-amino-1,2,4-triazole

acetonitrile

Allyl bromide

→

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

용매

ethyl alcohol

반응 조건

후처리

1. 1
   workup.STIRRINGto stir for five days at ambient temperature, whereupon it
2. 2
   여과was filtered
3. 3
   기타transferred to a large round bottomed flask
4. 4
   기타The solvent and excess allyl bromide were rotary evaporated away
5. 5
   기타leaving a viscous yellow oil
6. 6
   기타resulting in a large crop of fine needles
7. 7
   여과The needles were filtered away
8. 8
   세척washed with cold isopropyl alcohol
9. 9
   기타cold diethyl ether, transferred to a preweighed Schlenk flask
10. 10
    기타vacuum dried overnight

실험 절차

4-amino-1,2,4-triazole, 10.000 g, 118 mmoles, was dissolved into 200 ml of fresh acetonitrile and stirred vigorously. Allyl bromide, 43.10 g, 356 mmoles, was added slowly to the solution at room temperature. The reaction mixture was protected from light and allowed to stir for five days at ambient temperature, whereupon it was filtered, and transferred to a large round bottomed flask. The solvent and excess allyl bromide were rotary evaporated away leaving a viscous yellow oil. The oil was dissolved in a minimum amount of ethyl alcohol and the resultant clear, yellow solution layered with diethyl ether, and stored at 4° C. for 24 hours, resulting in a large crop of fine needles. The needles were filtered away washed with cold isopropyl alcohol and then cold diethyl ether, transferred to a preweighed Schlenk flask and vacuum dried overnight to leave a fluffy crystalline product of 1-allyl-4-amino-1,2,4-triazolium bromide in decent yield 12.657 g, 62 mmoles. Melting point: 59-62° C.; DSC onset: 130° C.

출처