反応 #3119

ord-065831d99277499b89b8f6f92e86ad30

反応条件

温度
230°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the mixture was reacted
  2. 2
    その他After the reaction
  3. 3
    温度the system was cooled to room temperature
  4. 4
    ろ過insoluble matters were filtered
  5. 5
    その他the filtrate was purified by silica gel column chromatography

実験手順

In a 100 ml-volume flask, 6 g of 3,4-xylidine, 34 g of ethyl 3-iododihydrocinnamate, 19 g of potassium carbonate, 5 g of copper sulfate pentahydrate and 20 ml of n-tridecane were placed, and the mixture was reacted under heating at 230° C. for 10 hours 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 20 g of N, N-bis[3-(2-ethoxycarbonylethyl)phenyl]-3,4-xylidine as an oily substance. The IR spectrum of the product is shown in FIG. 1.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05731118uspto-grants-1998_03