Reaktion #47843

ord-850aa1a6feec4aa5a9012bc8bff7fe18

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturby refluxing for 6 hrs
  2. 2
    WaschenThe resulting mixture washed with saturated saline
  3. 3
    Extraktionextracted with ethyl acetate
  4. 4
    SonstigeThe organic layer was separated
  5. 5
    Trocknendried over anhydrous MgSO4
  6. 6
    Einengenconcentrated under a reduced pressure
  7. 7
    SonstigeThe resulting residue was purified by flash chromatography

Vorschrift

1-Bromo-6-methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (120 mg, 0.32 mmol) obtained in Example 18 was dissolved in THF (10 mL), and benzylamine (102.87 mg, 0.11 mL, 0.93 mmol) and sodium iodide (9.60 mg, 0.06 mmol) were added thereto, followed by refluxing for 6 hrs. The resulting mixture washed with saturated saline and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 56 mg of the titled compound (yield: 44%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745439B2uspto-grants-2010_06