Reaktion #60790

ord-c19045a302f14666847a11bd7e283cf0

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONIce was added to the cooled mixture, which
  2. 2
    Filtrationthe resultant precipitate filtered off
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigedried at 60° C. in vacuo

Vorschrift

Phosphorous pentoxide (1.06 g) was added to N-(4,6diaminopyrimidin-5-yl)-1-methyl-4-phenyl-1H-imidazole-5-carboxamide (intermediate 7) (171 mg) followed by phosphoric acid (85%, 0.76 mL) and heated at 160° C. for 72 hours. Ice was added to the cooled mixture, which was then adjusted to pH 5 with aqueous NH3, the resultant precipitate filtered off, washed with water and dried at 60° C. in vacuo to give the title compound as a cream solid (156 mg, 89%);

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07427616B2uspto-grants-2008_09