반응 #83182

반응 방정식

alpha-(4-chlorophenyl)-alpha-ethyl-1H-1,2,4-triazole-1-propanenitrile

sodium hydroxide

→

white solid

수율 91.6%

2-(4-chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]butyramide

수율 91.6%

용매

dimethyl sulfoxide

반응 조건

후처리

1. 1
   기타was consumed
2. 2
   workup.ADDITIONThe reaction was poured into water
3. 3
   추출extracted with ethyl acetate
4. 4
   세척After washing with brine
5. 5
   건조the organic phase was dried over magnesium sulfate
6. 6
   농축concentrated under vacuum
7. 7
   온도without heating
8. 8
   기타Removal of the solvent
9. 9
   기타gave a foamy glassy solid which
10. 10
    기타was triturated with hexane
11. 11
    여과filtered

실험 절차

To a 500 mL flask was charged 100.0 g (0.38 mole) of alpha-(4-chlorophenyl)-alpha-ethyl-1H-1,2,4-triazole-1-propanenitrile and 100 mL of dimethyl sulfoxide. To the stirring solution was added 100 g (1.25 mole) of 50% sodium hydroxide. The reaction mixture was heated at 100° C. for 1 hour after which GLC indicated the starting material was consumed. The reaction was poured into water and extracted with ethyl acetate. After washing with brine, the organic phase was dried over magnesium sulfate and concentrated under vacuum without heating. Removal of the solvent gave a foamy glassy solid which was triturated with hexane, filtered and gave 97 g (91% yield) of a white solid, melting point 139°-140° C.

출처