تفاعل #812915

ord-70c7a09973e04d0dabe5fc3e682d3bf3

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىreaction at a temperature of 190° to 220° C. for 12 hours
  2. 2
    استخلاصThe reaction product was then extracted with 70 ml of toluene
  3. 3
    أخرىThe insoluble contents were removed by filtration
  4. 4
    تركيزThe filtrate was then concentrated
  5. 5
    أخرىto obtain an oily material
  6. 6
    أخرىThe crude product thus obtained
  7. 7
    أخرىwas then purified by column chromatography (carrier: silica gel; elute: 1/6 mixture of toluene and n-hexane)

الإجراء التجريبي

17.6 g (0.078 mol) of N-phenyl-p-isobutylaniline, 12.6 g (0.031 mol) of 4,4'-diiodobiphenyl, 12.9 g (0.093 mol) of anhydrous potassium carbonate, and 0.89 g (0.014 mol) of copper powder were mixed. The mixture was then allowed to undergo reaction at a temperature of 190° to 220° C. for 12 hours. The reaction product was then extracted with 70 ml of toluene. The insoluble contents were removed by filtration. The filtrate was then concentrated to obtain an oily material. The crude product thus obtained was then purified by column chromatography (carrier: silica gel; elute: 1/6 mixture of toluene and n-hexane) to obtain 8.5 g (yield: 45.7%) of N,N'-bis(p-isobutylphenyl)-N,N'-diphenylbenzidine. The melting point of the product was from 133.8° C. to 135.3° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05707747uspto-grants-1998_01