Reaktion #1451701

ord-5290af3b1fce4d54aa5d3f5df2b8bb97

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturA heavy walled, sealable tube suitable for microwave heating
  2. 2
    Sonstigehad reacted (15 minutes)
  3. 3
    SonstigeThe tube was sealed
  4. 4
    Temperaturthen cooled
  5. 5
    SonstigeThe precipitate was collected
  6. 6
    Waschenwashed with water until pH=7
  7. 7
    Sonstigedried 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07888374B2uspto-grants-2011_02