تفاعل #342136

ord-f4878c6c5b1d4a9ca85ffee38765a8b7

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىPrecipitate formed in the reaction tube
  2. 2
    درجة الحرارةafter heating
  3. 3
    أخرىthe reaction at 75° C. for 1 hr
  4. 4
    أخرىthe solvent was evaporated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
  6. 6
    أخرىprecipitated by the addition of hexanes
  7. 7
    أخرىThe resulting solid was isolated by filtration
  8. 8
    أخرىdried

الإجراء التجريبي

4-(3-phenylphenylhydrazono)-4H-pyrazole-3,5-diamine was prepared using 123 mg (0.5 mmol) of 2-[(biphenyl-2-yl)hydrazono]malononitrile, which was derived from 2-aminobiphenyl (169 mg, 1.0 mmol) and malononitrile (1.5 mmol), and hydrazine hydrate. Precipitate formed in the reaction tube immediately after the addition of the hydrazine hydrate then the solution cleared. Very little solid remained after heating the reaction at 75° C. for 1 hr, however, analysis of the reaction solution by TLC indicated that no starting material remained. The solution was allowed to cool to ambient temperature and the solvent was evaporated. The residue was dissolved in ethyl acetate and then precipitated by the addition of hexanes. The resulting solid was isolated by filtration and dried to yield 85 mg (61%) of the compound as an orange solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07875728B2uspto-grants-2011_01