تفاعل #812925

ord-ecc07d61f69b4bf5be8ba6a6c6e8dfa6

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىreaction at a temperature of 190° C. to 205° C. for 10 hours
  2. 2
    استخلاصThe reaction product was then extracted with 200 ml of toluene
  3. 3
    أخرىThe insoluble contents were then removed by filtration
  4. 4
    تركيزThe filtrate was then concentrated to dryness
  5. 5
    أخرىThe concentrate was then purified by column chromatography (carrier: silica gel; elute: 6/1 mixture of toluene and ethyl acetate)

الإجراء التجريبي

20.0 g (0.15 mol) of acetanilide, 65.0 g (0.16 mol) of 4,4'-diiodobiphenyl, 22.1 g (0.16 mol) of anhydrous potassium carbonate, 2.16 g (0.034 mol) of copper powder, and 35 ml of nitrobenzene were mixed. The reaction mixture was then allowed to undergo reaction at a temperature of 190° C. to 205° C. for 10 hours. The reaction product was then extracted with 200 ml of toluene. The insoluble contents were then removed by filtration. The filtrate was then concentrated to dryness. The concentrate was then purified by column chromatography (carrier: silica gel; elute: 6/1 mixture of toluene and ethyl acetate) to obtain 40.2 g (yield: 64.8%) of N-(4'-iodo-4-biphenylyl)acetanilide. The melting point of the product was from 135.0° C. to 136.0 ° C.

المصدر

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