Reaktion #452482

ord-81caef4093fa442c9c32575e3bed6bc2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  2. 2
    workup.ADDITIONWater was added to the residue
  3. 3
    WaschenAfter the resulting mixture was washed three times with ethyl ether, sodium chloride
  4. 4
    workup.ADDITIONwas added to the water layer
  5. 5
    Extraktionfollowed by extraction four times with chloroform-methanol (2:1)
  6. 6
    WaschenThe extract was washed with an aqueous solution of sodium chloride
  7. 7
    Trocknendried over anhydrous magnesium sulfate
  8. 8
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

After a mixture consisting of 2-chloromethyl-quinoline hydrochloride (63.16 g, 295 mmol), triethyl-amine (29.85 g, 295 mmol), homopiperazine (50.08 g, 591 mmol) and ethanol (600 ml) was stirred at room temperature for 2 days, the solvent was distilled off under reduced pressure. Water was added to the residue. After the resulting mixture was washed three times with ethyl ether, sodium chloride was added to the water layer, followed by extraction four times with chloroform-methanol (2:1). The extract was washed with an aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, whereby 28.00 g of the title compound were obtained as a yellow oil (yield: 39.3%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06127360uspto-grants-2000_10