Reaktion #40983

ord-e9f8b59231f648d7990315cef63ab5fc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITwas continued for 48 hours
  3. 3
    Extraktionthe product was extracted with ethyl acetate
  4. 4
    TrocknenThe organic phase was dried (Na2SO4)
  5. 5
    Sonstigeevaporated
  6. 6
    SonstigeThe crude was triturated with iPr2O

Vorschrift

A mixture of 5-(6-Fluoro-pyridin-2-yl)-1H-pyrimidine-2,4-dione hydrochloride (Prep75, 200 mg, 0.82 mmol), and K2CO3 (169 mg, 1.23 mmol) in DMF (4 ml) was stirred 1 hour at room temperature. 3-Bromo-1,1dimethoxy-propane (165 mg, 0.90 mmol) was added and stirring was continued for 48 hours. Water (50 ml) was added and the product was extracted with ethyl acetate. The organic phase was dried (Na2SO4) and evaporated. The crude was triturated with iPr2O to give 179 mg of the final compound as a white solid (70% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727988B2uspto-grants-2010_06