Reaktion #60738

ord-fd4558891c2746bcb49800b4bddd4e77

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas cooled to 0 C
  2. 2
    Sonstigethe reaction was quenched by slow addition of water and 1 N sodium hydroxide
  3. 3
    FiltrationThe biphasic mixture was filtered through a pad of diatomaceous earth
  4. 4
    Einengenthe filtered solution was concentrated to dryness

Vorschrift

To a solution of 1-(4-isopropylpiperazin-1-yl)-4-phenylbutane-1,4-dione 4-oxime (625 mg, 2.0 mmol) in 10 mL of THF was slowly added lithium aluminum hydride (250 mg, 6.6 mmol). The reaction flask was heated at 70° C. for 4 h after which time the flask was cooled to 0 C and the reaction was quenched by slow addition of water and 1 N sodium hydroxide. The biphasic mixture was filtered through a pad of diatomaceous earth, and the filtered solution was concentrated to dryness to afford 536 mg (98%) of the title compound as a crude residue that was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07427632B2uspto-grants-2008_09