Reacción #4220

Ecuación de reacción

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

Rendimiento 65.0%

Disolventes

ethanol

Condiciones de reacción

Tratamiento posterior

1. 1
   ConcentraciónThe mixture was then concentrated
2. 2
   Temperaturathe ethyl acetate mixture was heated
3. 3
   TemperaturaIt was then cooled in an ice bath
4. 4
   Filtraciónthe solid was filtered off
5. 5
   Lavadorinsed with ethyl acetate
6. 6
   ConcentraciónThe filtrate was concentrated
7. 7
   workup.DISSOLUTIONthe residue was dissolved in ether/hexane
8. 8
   FiltraciónThe precipitate was filtered off
9. 9
   Lavadorinsed with ether
10. 10
    Otrothe free base was obtained

Procedimiento

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.

Fuente