Reaktion #4272

ord-a11989da57094792a3813bfd266f2693

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA clear solution is obtained at first, which
  2. 2
    SonstigeA fine crystal slurry is precipitated which
  3. 3
    Temperaturis cooled
  4. 4
    Filtrationsuction filtered
  5. 5
    Waschenwashed with 50 ml of absolute ethanol and 150 ml of acetone

Vorschrift

28 g (0.067 mol) of 5,11-dihydro-11-[1-oxo-2-methyl-6-(4-methyl-1-piperazinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one are suspended in 350 ml of absolute ethanol and 45 ml of ethereal hydrochloric acid are added with stirring at boiling temperature. A clear solution is obtained at first, which goes cloudy again after some time. A fine crystal slurry is precipitated which is cooled and suction filtered and then washed with 50 ml of absolute ethanol and 150 ml of acetone.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04724236uspto-grants-1988_02