Reaktion #41023

ord-8a7008fcf016486bb7b985cf8340c0ce

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe mixture was extracted with ethyl acetate
  2. 2
    TrocknenThe organic phase was dried (Na2SO4)
  3. 3
    Filtrationfiltered
  4. 4
    Sonstigeevaporated
  5. 5
    SonstigeThe crude was purified by flash chromatography
  6. 6
    Wascheneluting with DCM-MeOH—NH4OH (98-2-0.2)

Vorschrift

A mixture of 5-pyrazin-2-yl-1H-pyrimidine-2,4-dione hydrochloride (Prep125, 2.19 mmol), and K2CO3 (302 mg, 2.19 mmol) in DMF (20 ml) was stirred 30 minutes at room temperature. 90% 3-Bromo-1,1dimethoxy-propane (365 μl, 2.41 mmol) was added in two portions during 2 days. Water was added and the mixture was extracted with ethyl acetate. The organic phase was dried (Na2SO4), filtered and evaporated. The crude was purified by flash chromatography eluting with DCM-MeOH—NH4OH (98-2-0.2) to give 221 mg of the title compound (35% yield).

Quelle

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