Reaktion #78061

ord-791c61bd4d46488d9cd3f88bc69b7774

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAn organic phase was separated
  2. 2
    Extraktionan aqueous phase was extracted with dichloromethane
  3. 3
    TrocknenA combined organic phase was dried over magnesium sulfate
  4. 4
    Sonstigethe solvents were removed under reduced pressure
  5. 5
    SonstigeAfter crystallization from diisopropyl ether and n-hexane

Vorschrift

To a suspension of 1-acetyl-4-aminopiperidine hydrochloride (536 mg) in dichloromethane (5 ml) were added 4-fluorophenyl isocyanate (375 μl) and diisopropylethylamine (575 μl ) at ambient temperature. After stirring for 3 hours, the reaction mixture was diluted with dichloromethane. An organic phase was separated and an aqueous phase was extracted with dichloromethane. A combined organic phase was dried over magnesium sulfate and the solvents were removed under reduced pressure. After crystallization from diisopropyl ether and n-hexane, N-(1-acetylpiperidin-4-yl)-N′-(4-fluorophenyl)urea (448 mg) was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06710043B1uspto-grants-2004_03