تفاعل #812917

ord-de9d3efeb1d849038534198786c197f0

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىreaction at a temperature of 210° to 225° 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: 1/4 mixture of toluene and n-hexane)

الإجراء التجريبي

8.1 g (0.036 mol) of N-phenyl-p-tertiarybutylaniline, 7.3 g (0.018 mol) of 4,4'-diiodobiphenyl, 7.5 g (0.054 mol) of anhydrous potassium carbonate, and 0.53 g (0.008 mol) of copper powder were mixed. The mixture was then allowed to undergo reaction at a temperature of 210° to 225° 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: 1/4 mixture of toluene and n-hexane) to obtain 4.5 g (yield: 41.7%) of N,N'-bis(p-tertiarybutylphenyl)-N,N'-diphenylbenzidine. The melting point of the product was from 232.2° C. to 232.6° C.

المصدر

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