Reaktion #456616

ord-23b495d70d31451db579e31d34946c0d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxing
  2. 2
    EinengenThe reaction mixture was concentrated under reduced pressure
  3. 3
    workup.ADDITIONChloroform was added to the residue
  4. 4
    Sonstigean insoluble matter was removed
  5. 5
    EinengenThe filtrate was concentrated under reduced pressure
  6. 6
    SonstigeThe residue was purified by chromatography on a silica gel column (ethyl acetate:methanol=5:1), whereby the title compound

Vorschrift

3-(3-Chloropropoxy)-6-ethoxycarbonylflavone (1.2 mmol), 1-(2-quinolinylmethyl)piperazine (0.32 g, 1.2 mmol), sodium hydrogencarbonate (0.31 g, 2.9 mmol) and sodium iodide (0.43 g, 2.9 mmol) were dissolved in 25 ml of 2-butanone, followed by overnight refluxing. The reaction mixture was concentrated under reduced pressure. Chloroform was added to the residue, and an insoluble matter was removed. The filtrate was concentrated under reduced pressure. The residue was purified by chromatography on a silica gel column (ethyl acetate:methanol=5:1), whereby the title compound represented by the following formula was obtained as a brown oil (yield: 75%). ##STR64##

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06136848uspto-grants-2000_10