Reaktion #1369350

ord-a940852c62624a69ae773e7e9b6edebe

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    Extraktionextracted with ethyl acetate (100 ml)
  3. 3
    WaschenThe extract was washed with saturated brine
  4. 4
    Trocknendried over anhydrous sodium sulfate
  5. 5
    SonstigeThe solvent was evaporated
  6. 6
    Sonstigethe obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:hexane=1:1)

Vorschrift

To a 20% dimethylamine-ethanol solution (15.4 g) of 2,4-dichloropyrimidine (3.0 g) was added triethylamine (3 ml) under ice-cooling, and the mixture was stirred for 30 min. The reaction mixture was poured into water (100 ml) and extracted with ethyl acetate (100 ml). The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:hexane=1:1) to give the title compound (1.90 g) as white crystals, m.p.=77-79° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06455528B1uspto-grants-2002_09