Reaktion #11570

ord-7c9faa00da474823a42f76ed03b4aa2b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated under reduced pressure
  2. 2
    Waschenthe precipitated solid was washed with ethyl acetate
  3. 3
    Filtrationfiltered off
  4. 4
    SonstigeThe obtained crude crystals
  5. 5
    Sonstigewere recrystallized from 2-butanone (5.0 ml)

Vorschrift

A 4 N solution of hydrogen chloride in ethyl acetate (0.400 ml, 1.60 mmol) was added to a solution of 1-[2-(1-adamantyl)ethyl]-1-pentyl-3-[3-(4-pyridyl)propyl]urea (Compound No. 1-1) (200 mg, 0.486 mmol) in chloroform (0.3 ml). The solvent was evaporated under reduced pressure, and the precipitated solid was washed with ethyl acetate and filtered off. The obtained crude crystals were recrystallized from 2-butanone (5.0 ml) to give 94 mg (43%) of the titled compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098226B2uspto-grants-2006_08