Reaktion #449376
ord-3efc76301fb44042b4cd101b21943b90
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstige(approximately one minute)
- 2TemperaturThe reaction mixture was cooled
- 3workup.WAITplaced in an ice bath for a half hour
- 4FiltrationThe crystallized product was filtered
- 5Waschenwashed well with diethyl ether, and air
- 6Sonstigedried
Vorschrift
4-Amino-3-pyridinol (3.3 g) was added to 1-piperidinylformamide dimethyl acetal (50 ml) and the mixture was stirred at 100° C. until it became homogeneous (approximately one minute). The reaction mixture was cooled, and placed in an ice bath for a half hour. The crystallized product was filtered, washed well with diethyl ether, and air dried to yield 4.64 g of product. This was recrystallized from ethyl acetate and dried under high vacuum and refluxing ethanol overnight to yield 3.39 g of fluffy needles, m.p. 171°-172.5° C.