Reaktion #742249

ord-6341323ae66147b3b237f867cf3338d6

Reaktionsgleichung

CCOC(=O)C=P(c1ccccc1)(c1ccccc1)c1ccccc1
ethoxycarbonylmethylenetriphenylphosphorane
Cc1ccccc1
toluene
CCN(CC)c1ccc(C(C)=O)c(O)c1
1-(4-diethylamino-2-hydroxy-phenyl)ethanone
CCOC(=O)C=C(C)c1ccc(N(CC)CC)cc1O
3(4-Diethylamino-2-hydroxy-phenyl)-but-2-enoic acid ethyl ester

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThen the reaction mixture was heated to reflux
  2. 2
    TemperaturAfter refluxing for 31 hours the mixture
  3. 3
    Temperaturwas cooled down
  4. 4
    Sonstigeevaporated to dryness
  5. 5
    SonstigeThe resulting dark oil was purified by chromatography
  6. 6
    Sonstigeto yield a colourless oil

Vorschrift

To a suspension of 5.27 g ethoxycarbonylmethylenetriphenylphosphorane in 10 ml of toluene, a solution of 2.02 g 1-(4-diethylamino-2-hydroxy-phenyl)ethanone (DE 28 44 606) was dropped in at room temperature. Then the reaction mixture was heated to reflux. After refluxing for 31 hours the mixture was cooled down and evaporated to dryness. The resulting dark oil was purified by chromatography to yield a colourless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE043006E1uspto-grants-2011_12