Reaktion #47817

ord-3c1bf3a9f67045bab896a8932ac5a56e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxed for 24 hrs
  2. 2
    WaschenThe resulting mixture washed with sodium bicarbonate
  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
    SonstigeThen, the resulting residue was purified by flash chromatography

Vorschrift

1-Oxo-3-phenyl-6-(3-phenylpropoxy)-1H-indene-2-carboxylic acid ethyl ester (2 g, 4.85 mmol) obtained in Example 7 was dissolved in methanol, p-toluenesulfonic acid (92 mg, 0.49 mmol) was added thereto, and refluxed for 24 hrs. The resulting mixture washed with sodium bicarbonate and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. Then, the resulting residue was purified by flash chromatography to obtain 1.2 g of the titled compound (yield: 62%).

Quelle

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