反应 #83182
ord-2ab817c46ab84773bbd4994ae55649d7
反应方程式
反应条件
温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他was consumed
- 2workup.ADDITIONThe reaction was poured into water
- 3萃取extracted with ethyl acetate
- 4洗涤After washing with brine
- 5干燥the organic phase was dried over magnesium sulfate
- 6浓缩concentrated under vacuum
- 7温度without heating
- 8其他Removal of the solvent
- 9其他gave a foamy glassy solid which
- 10其他was triturated with hexane
- 11过滤filtered
实验过程
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.