반응 #4220

반응 방정식

2-(4-chlorophenoxy-methyl)-2-tert.-butyl-oxirane

1,2,4-triazole

ethyl acetate

→

2-(4-chlorophenoxy-methyl)-3,3-dimethyl-1-(1,2,4-triazol-1yl)butan-2-ol

수율 65.0%

용매

ethanol

반응 조건

후처리

1. 1
   농축The mixture was then concentrated
2. 2
   온도the ethyl acetate mixture was heated
3. 3
   온도It was then cooled in an ice bath
4. 4
   여과the solid was filtered off
5. 5
   세척rinsed with ethyl acetate
6. 6
   농축The filtrate was concentrated
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ether/hexane
8. 8
   여과The precipitate was filtered off
9. 9
   세척rinsed with ether
10. 10
    기타the free base was obtained

실험 절차

72.15 g (0.3 mole) of 2-(4-chlorophenoxy-methyl)-2-tert.-butyl-oxirane and 24.15 g (0.35 mole) of 1,2,4-triazole were heated under reflux in 120 ml of ethanol for 48 hours. The mixture was then concentrated, the residue was taken up in 200 ml of ethyl acetate and the ethyl acetate mixture was heated. It was then cooled in an ice bath and the solid was filtered off and rinsed with ethyl acetate. The filtrate was concentrated, the residue was dissolved in ether/hexane and the solution was gassed with hydrogen chloride. The precipitate was filtered off and rinsed with ether and the free base was obtained by adding ethyl acetate/1N sodium hydroxide solution. 60.2 g (65% of theory) of 2-(4-chlorophenoxy-methyl)-3,3-dimethyl-1-(1,2,4-triazol-1yl)butan-2-ol of melting point 84°-87° C. were obtained.

출처