Reaktion #77672

ord-63af00af25dc450f9038d63a2aa45ae1

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to room temperature
  2. 2
    Einengenconcentrated in vacuo
  3. 3
    Filtrationthe mixture was then filtered

Vorschrift

In a round-bottomed flask, 4-(4-fluoro-phenyl)-4-oxo-butyric acid (4.90 g, 25.0 mmol) and hydrazine hydrate (1.70 ml, 35.0 mmol) were dissolved in ethanol (50 ml), and the reaction mixture was heated to about 80° C. for about ninety minutes. The mixture was allowed to cool to room temperature and then concentrated in vacuo. The resulting solids were suspended and stirred in ethanol (10 ml) for ten minutes and the mixture was then filtered to give pure product (4.14 g, 21.5 mmol, 86% yield). LRMS ([M+H]+)=193.2; m.p. 191-193° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06706743B2uspto-grants-2004_03