Reaktion #2396980
ord-a117a67ff8e04619bbe854469e31a3bf
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated
- 2Temperaturto reflux for two hours
- 3Temperaturreflux
- 4TemperaturAfter cooling
- 5Filtrationthe crystallized solid was collected by filtration
- 6Waschenwashed with ethanol
- 7Sonstigeto obtain
- 8Filtrationafter filtration
- 9Sonstigedrying
Vorschrift
A mixture of α-bromo-4-acetylpyridine hydrobromide (140.0 g, 0.50 mol) and potassium thiocyanate (53.4 g, 0.55 mol) in absolute ethanol (1500 mL) was heated to reflux for two hours. To the resulting mixture was added concentrated hydrochloric acid (250 mL) and water (500 mL) and reflux continued for five hours. After cooling, the crystallized solid was collected by filtration and washed with ethanol. The resulting material was suspended in water and neutralized with aqueous sodium bicarabonate to obtain, after filtration and drying, 2-hydroxy-4-(4-pyridyl)thiazole 39.0 g, 44%). mp. 250° C.