Reaktion #1451701
ord-5290af3b1fce4d54aa5d3f5df2b8bb97
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturA heavy walled, sealable tube suitable for microwave heating
- 2Sonstigehad reacted (15 minutes)
- 3SonstigeThe tube was sealed
- 4Temperaturthen cooled
- 5SonstigeThe precipitate was collected
- 6Waschenwashed with water until pH=7
- 7Sonstigedried under reduced pressure at 95° C.
Vorschrift
A heavy walled, sealable tube suitable for microwave heating was charged with 6 mL of 2-propanol and 150 mg (6.5 mmol) of sodium. The mixture was stirred at 95° C. until all of the sodium had reacted (15 minutes), then 650 mg (3.05 mmol) of 2-bromo-4,6-diaminonicotinonitrile was added. The tube was sealed, and the mixture was heated with a microwave apparatus at 150° C. for 10 minutes then cooled and diluted with 30 mL of water. The precipitate was collected, washed with water until pH=7, then dried under reduced pressure at 95° C. to provide 312 mg (53%) of pale yellow crystals.