Reaktion #53452

Reaktionsgleichung

Ethyl 8-bromo-1-[6-(t-butylamino)-3,5-difluoro-pyridin-2-yl]-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

hydrochloric acid

acetic acid

→

title compound

Ausbeute 95.2%

1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

Ausbeute 95.2%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated for 5 hours
2. 2
   Temperaturreflux
3. 3
   Temperaturto cool down
4. 4
   FiltrationThe precipitate was collected by filtration
5. 5
   Waschenwashed successively with ethanol and diisopropyl ether in this order

Vorschrift

Ethyl 8-bromo-1-[6-(t-butylamino)-3,5-difluoro-pyridin-2-yl]-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate (1.38 g) was added to a liquid mixture of 12% hydrochloric acid (3.5 mL) and acetic acid (3.5 mL), and the mixture was heated for 5 hours under stirring and reflux. Subsequent to addition of distilled water (5 mL), the mixture was allowed to cool down. The precipitate was collected by filtration, and washed successively with ethanol and diisopropyl ether in this order to obtain the title compound (1.10 g) as a colorless powder.

Quelle