Reaktion #518698

ord-122515e4d47b4be585bfc5272c6ea2dd

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvents were removed in vacuo
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in acetic acid
  3. 3
    Sonstigeagain evaporated to dryness
  4. 4
    SonstigeThe resinous residue was triturated with diethyl ether
  5. 5
    FiltrationAfter filtration 90 mg of a colourless amorphous powder
  6. 6
    Sonstigewere obtained

Vorschrift

117 mg (0.19 mmol) of the product obtained in step c) were dissolved in 5 ml of dichloromethane and stirred for 3 hours with 1 ml of trifluoroacetic acid under an inert gas atmosphere at room temperature. The solvents were removed in vacuo, and the residue was dissolved in acetic acid and again evaporated to dryness. This procedure was repeated once. The resinous residue was triturated with diethyl ether. After filtration 90 mg of a colourless amorphous powder were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06660728B2uspto-grants-2003_12