Reaktion #4220

Reaktionsgleichung

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

Ausbeute 65.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe mixture was then concentrated
2. 2
   Temperaturthe ethyl acetate mixture was heated
3. 3
   TemperaturIt was then cooled in an ice bath
4. 4
   Filtrationthe solid was filtered off
5. 5
   Waschenrinsed with ethyl acetate
6. 6
   EinengenThe filtrate was concentrated
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ether/hexane
8. 8
   FiltrationThe precipitate was filtered off
9. 9
   Waschenrinsed with ether
10. 10
    Sonstigethe free base was obtained

Vorschrift

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.

Quelle