Reaktion #157309
ord-19e6337ddada4661bb84eebb88a950a1
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturto reflux overnight
- 2Einengenthe reaction mixture was concentrated under reduced pressure
- 3Filtrationcollected by filtration
- 4Waschenwashed with water (2×)
- 5Sonstigeair-dried
- 6SonstigeFurther drying in a 35° C. vacuum oven
Vorschrift
3-Hydroxy-2-aminopyridine (2.00 g, 18.2 mmol) and potassium hydroxide (1.22 g, 21.8 mmol) were dissolved in carbon disulfide (15 mL) and EtOH (25 mL), and the reaction mixture was heated to reflux overnight. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The resulting solid was suspended in 1 M aqueous HCl, collected by filtration, washed with water (2×) and air-dried. Further drying in a 35° C. vacuum oven gave 2.52 g (91%) of the title compound as a tan solid. LC-MS: RT=4.82 min., [M+H]+=153.1