تفاعل #1809802

ord-c87ce3e7d72c4d30b0f44fd3f67bc4a2

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux for two hours
  3. 3
    أخرىresulting in a crude orange product which
  4. 4
    أخرىwas isolated by filtration
  5. 5
    غسيلThe product was then washed with ether
  6. 6
    أخرىdried
  7. 7
    أخرىThe product was purified further
  8. 8
    درجة الحرارةat refluxing temperature
  9. 9
    ترشيحfiltering the slurry
  10. 10
    أخرىto recover the dye
  11. 11
    أخرىwas above 310° C

الإجراء التجريبي

A slurry composed of 1-(4-carboxyphenyl)-3-methyl-2-pyrazolin-5-one (21.8 g, 0.10 mol), 4-dimethylamino-benzaldehyde (14.9 g, 0.10 mol) and EtOH (250 ml) was heated at reflux for two hours. The reaction mixture was cooled to room temperature, resulting in a crude orange product which was isolated by filtration. The product was then washed with ether and dried. The product was purified further by making a slurry of the solid in EtOH (700 ml) at refluxing temperature and filtering the slurry to recover the dye. The treatment was repeated. The mp of the product was above 310° C. The NMR and IR spectra were consistent with the structure assigned. The C, H, and N elemental analyses were in agreement with those calculated for the empirical formula.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04857446uspto-grants-1989_08