تفاعل #687298

ord-2828f1bfc8204a1cb64c33bceacd85d3

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىfollowed by reaction at 190 to 205° C. for 10 hours
  2. 2
    استخلاصThe reaction product was extracted with 200 ml of toluene
  3. 3
    أخرىthe insoluble matter was removed by filtration
  4. 4
    تركيزThen, the filtrate was concentrated to dryness
  5. 5
    أخرىThe resulting solid matter was purified by column chromatography (carrier: silica gel, eluate: toluene/ethyl acetate=6/1)

الإجراء التجريبي

There were mixed 20.3 g (0.15 mole) of acetanilide, 73.1 g (0.18 mole) of 4,4′-diiodobiphenyl, 22.1 g (0.16 mole) of anhydrous potassium carbonate, 2.16 g (0.034 mole) of copper powder and 35 ml of n-dodecane, followed by reaction at 190 to 205° C. for 10 hours. The reaction product was extracted with 200 ml of toluene, and the insoluble matter was removed by filtration. Then, the filtrate was concentrated to dryness. The resulting solid matter was purified by column chromatography (carrier: silica gel, eluate: toluene/ethyl acetate=6/1) to obtain 40.2 g (yield: 64.8%) of N-(4′-iodobiphenylyl)acetanilide. The melting point was 135.0 to 136.0° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07897816B2uspto-grants-2011_03