Reaktion #1479008

ord-2f4171afb6a849e791d7deaa37561f64

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resultant reaction mixture
  2. 2
    Einengenwas concentrated under reduced pressure
  3. 3
    workup.ADDITIONa mixture of chloroform and methanol (20:1)
  4. 4
    workup.ADDITIONwas added to the resultant residue
  5. 5
    FiltrationThe thus-precipitated crystals were filtered
  6. 6
    Sonstigethe resultant crystals were recrystallized from water

Vorschrift

Compound 3 (200 mg, 0.53 mmol) was dissolved in methanol (7.00 ml), and 28% aqueous ammonia (5.00 ml) was added to the resultant solution, followed by stirring at room temperature for four hours. The resultant reaction mixture was concentrated under reduced pressure, and a mixture of chloroform and methanol (20:1) was added to the resultant residue. The thus-precipitated crystals were filtered, and then the resultant crystals were recrystallized from water, to thereby yield compound 4 (113 mg, 0.39 mmol, 73.6%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07339053B2uspto-grants-2008_03