Reaktion #46917

ord-bfcda754581f492fbdf500441de8d793

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 24 hours
  2. 2
    TemperaturUpon cooling
  3. 3
    Filtrationthe mixture was filtered over diatomaceous earth
  4. 4
    Einengenconcentrated
  5. 5
    SonstigeThe residue was purified by chromatography with DCM

Vorschrift

A mixture of 2,4′-dibromoacetophenone (3.0 g, 10.8 mmol), ethyl acetoacetate (1.48 mL, 10.8 mmol) and potassium carbonate (4.5 g, 32.4 mmol) were heated in 2-butanone (50 mL) at reflux for 24 hours. Upon cooling, the mixture was filtered over diatomaceous earth and concentrated. The residue was purified by chromatography with DCM to provide the title compound as an oil. 1H NMR (CDCl3) δ ppm 1.30 (3H), 2.10 (3H), 3.19 (2H), 3.75 (1H), 4.15 (2H), 7.50 (2H), 7.81 (2H); MS (ESI) m/z 326/328.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741364B2uspto-grants-2010_06