تفاعل #83182

ord-2ab817c46ab84773bbd4994ae55649d7

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas consumed
  2. 2
    workup.ADDITIONThe reaction was poured into water
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلAfter washing with brine
  5. 5
    تجفيفthe organic phase was dried over magnesium sulfate
  6. 6
    تركيزconcentrated under vacuum
  7. 7
    درجة الحرارةwithout heating
  8. 8
    أخرىRemoval of the solvent
  9. 9
    أخرىgave a foamy glassy solid which
  10. 10
    أخرىwas triturated with hexane
  11. 11
    ترشيحfiltered

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05624916uspto-grants-1997_04