Reaktion #711744

ord-6fc374320c3840aba2337dfc60c25733

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was evaporated under vacuum
  2. 2
    Sonstigethe residue partitioned between DCM (20 mL) and 1M HCl (20 mL)
  3. 3
    SonstigeThe phases were separated
  4. 4
    Waschenthe organic phase was washed with water (2×20 mL)
  5. 5
    Sonstigeevaporate under vacuum

Vorschrift

A mixture of 6-(bromomethyl)-5-(3-chlorobenzoyl)-1,3-dimethylpyrimidine-2,4(1H,3H)-dione (2 g, 5.38 mmol), (R)-3-aminopropane-1,2-diol (0.490 g, 5.38 mmol) and triethylamine (0.750 ml, 5.38 mmol) in EtOH (17.94 ml) was heated under microwave irradiation at 100° C. for 1 hour. The mixture was evaporated under vacuum and the residue partitioned between DCM (20 mL) and 1M HCl (20 mL). The phases were separated and the organic phase was washed with water (2×20 mL). The organic phase was passed through a hydrophobic frit and evaporate under vacuum to afford the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09303035B2uspto-grants-2016_04