Reaktion #71401

Reaktionsgleichung

KOH

8-(2-fluoro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile

H2O

→

title compound

8-(2-Fluoro-3,5-dimethoxy-phenyl)-quinoxaline-5-carboxylic acid

Lösungsmittel

ethylene glycol

Et2O H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto cool to rt
2. 2
   Extraktionextracted with Et2O
3. 3
   workup.ADDITIONThe aqueous phase was acidified to pH 3 by addition of HCl
4. 4
   FiltrationThe resulting yellow solid was collected by vacuum filtration

Vorschrift

A solution of KOH (2.95 g, 52.7 mmol, 10 equiv) in H2O (20 mL) was added to 8-(2-fluoro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile (Step 94.2) (1.63 g mg, 5.3 mmol) in ethylene glycol (20 mL). The reaction mixture was stirred at 150° C. for 5 h, allowed to cool to rt, diluted with Et2O/H2O, and extracted with Et2O. The aqueous phase was acidified to pH 3 by addition of HCl. The resulting yellow solid was collected by vacuum filtration to provide 1.71 g of the title compound: ESI-MS: 329.1 [M+H]+; tR=4.18 min (System 1).

Quelle