Reaktion #9975

ord-d7ef2be036f64ada85c82b1e0ea6db93

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAt the end of this time, ethanol was removed by distillation under reduced pressure
  2. 2
    workup.ADDITIONTo the reaction residue was added water
  3. 3
    FiltrationThe precipitated crystals were collected by filtration

Vorschrift

5-Ethoxycarbonyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)thiophene (15.17 g (46.3 mmol), prepared as described in 1)) was dissolved in ethanol (150 ml). To the solution was added an aqueous solution of 1 N sodium hydroxide (93 ml, 93 mmol), and the resulting mixture was stirred at 100° C. for 30 minutes. At the end of this time, ethanol was removed by distillation under reduced pressure. To the reaction residue was added water, and then an aqueous solution of 1 N hydrochloric acid (93 ml). The precipitated crystals were collected by filtration, to give the title compound (12.64 g) as a pale brown powder (yield 91%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091352B2uspto-grants-2006_08