反应 #83182

ord-2ab817c46ab84773bbd4994ae55649d7

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他was consumed
  2. 2
    workup.ADDITIONThe reaction was poured into water
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤After washing with brine
  5. 5
    干燥the organic phase was dried over magnesium sulfate
  6. 6
    浓缩concentrated under vacuum
  7. 7
    温度without heating
  8. 8
    其他Removal of the solvent
  9. 9
    其他gave a foamy glassy solid which
  10. 10
    其他was triturated with hexane
  11. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05624916uspto-grants-1997_04