반응 #3120

ord-70576781abfa4a2db8a2ad21736fa5f6

반응 조건

온도
230°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the mixture was reacted
  2. 2
    기타After the reaction
  3. 3
    온도the system was cooled to room temperature
  4. 4
    여과insoluble matters were filtered
  5. 5
    기타the filtrate was purified by silica gel column chromatography

실험 절차

In a 100 ml-volume flask, 10.77 g of N,N'-diphenylbenzidine, 23.0 g of ethyl 3-iododihydrocinnamate, 11.61 g of potassium carbonate, 1.0 g of copper sulfate pentahydrate and 20 ml of n-tridecane were placed, and the mixture was reacted under heating at 230° C. for one hour in a nitrogen stream. After the reaction, the system was cooled to room temperature, the reaction mixture was dissolved in 50 ml of toluene, insoluble matters were filtered and the filtrate was purified by silica gel column chromatography using toluene to obtain 19.6 g of N,N'-diphenyl-N,N'-bis[3-(2-ethoxycarbonylethyl)phenyl]-[1,1'-biphenyl]-4,4'-diamine as an oily substance. The IR spectrum of the product is shown in FIG. 2.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05731118uspto-grants-1998_03