反応 #47703

ord-e3890998a6f74fe4bce322bc689e3077

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction mixtures
  2. 2
    その他to precipitate the dye
  3. 3
    ろ過The precipitate was filtered off
  4. 4
    洗浄washed with 3 times with 25 ml of ethyl acetate
  5. 5
    その他before being dried under vacuum until a constant weight
  6. 6
    その他was obtained
  7. 7
    その他1.09 g of orange powder were recovered

実験手順

0.800 g of N,N-diethyl-2-(3-formyl-1H-indol-1-yl)acetamide was solubilized in 4.2 ml of isopropanol. 0.238 g of piperidine was added, followed by 0.435 g of 2,3-dihydro-1H-indolizinium chloride dissolved in 7 ml of isopropanol. The reaction mixtures were brought to 80° C. for 24 h, with stirring. 50 ml of ethyl acetate were added in order to precipitate the dye. The precipitate was filtered off, and washed with 3 times with 25 ml of ethyl acetate before being dried under vacuum until a constant weight was obtained. 1.09 g of orange powder were recovered. The analyses were in conformity with the expected structure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07744658B2uspto-grants-2010_06