Reaktion #46158

ord-0ca0b1d62b744f8496166b2efb4398a0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    ExtraktionThe reaction mixture was extracted with ammonium chloride and ether
  2. 2
    Sonstigethe organic layer was separated
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigethe resulting residue was purified by column chromatography

Vorschrift

5-Chloromethyl benzo[1,3]dioxol (11.2 g, 65.7 mmol) was dissolved in Dimethylformamide. Then, potassium carbonate (18.2 g, 131.4 mmol), sodium iodide (10.8 g, 72.27 mmol) and ethyl benzoylacetate (12.5 ml, 72.27 mmol) were added thereto and stirred for 5 hours at room temperature. The reaction mixture was extracted with ammonium chloride and ether, the organic layer was separated, dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by column chromatography to obtain 2-benzo[1,3]dioxol-5-ylmethyl-3-oxo-3-phenylpropionate ethyl ester (16.4 g, 76%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741323B2uspto-grants-2010_06