Reaktion #63014

ord-48f8d9c6e4794a009e46c4eff477dccf

Reaktionsgleichung

COc1ccccc1C(C)=O
o-Methoxyacetophenone
CCO
ethanol
COc1ccccc1C(=O)C=O
(2-Methoxyphenyl)glyoxal

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture refluxed 21 hours
  2. 2
    workup.ADDITIONThe reaction mixture was treated with activated carbon
  3. 3
    Filtrationfiltered over diatomaceous earth
  4. 4
    Sonstigeto yield to an oil, 23.2 g
  5. 5
    workup.DISTILLATIONThe latter was distilled
  6. 6
    Sonstigeto yield
  7. 7
    Sonstigepurified title product, 8.4 g
  8. 8
    Temperaturon cooling

Vorschrift

SeO2 (12.4 g., 0.112 mol) was dissolved in 75 ml. of 95% ethanol by warming to 55°. o-Methoxyacetophenone (15.3 g., 0.102 mol) was added in one portion and the mixture refluxed 21 hours. The reaction mixture was treated with activated carbon, filtered over diatomaceous earth, and the filtrate stripped to yield to an oil, 23.2 g. The latter was distilled to yield purified title product, 8.4 g., bp 94°-96°/0.5 mm, which solidified on cooling.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04762921uspto-grants-1988_08