Reacción #83182
ord-2ab817c46ab84773bbd4994ae55649d7
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Otrowas consumed
- 2workup.ADDITIONThe reaction was poured into water
- 3Extracciónextracted with ethyl acetate
- 4LavadoAfter washing with brine
- 5Secadothe organic phase was dried over magnesium sulfate
- 6Concentraciónconcentrated under vacuum
- 7Temperaturawithout heating
- 8OtroRemoval of the solvent
- 9Otrogave a foamy glassy solid which
- 10Otrowas triturated with hexane
- 11Filtraciónfiltered
Procedimiento
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.