Reaktion #2164045

ord-939fb16311914604afed69f06abf23fd

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    TemperaturThe reaction mixture was cooled to near room temperature
  3. 3
    Waschenthe mixture was washed with a saturated sodium chloride aqueous solution three times
  4. 4
    TrocknenThe organic layers were dried over anhydrous magnesium sulfate
  5. 5
    Einengenconcentrated

Vorschrift

Into 4 ml of N,N-dimethylformamide was resolved 0.37 g of 4-(2-butynyloxy)-6-chloropyrimidine, 0.56 g of potassium carbonate and 0.2 g of 3,3-dimethylpyrrolidine was added therein, and the mixture was stirred for 6 hours at 80° C. The reaction mixture was cooled to near room temperature, ethyl acetate was added therein, and the mixture was washed with a saturated sodium chloride aqueous solution three times. The organic layers were dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.11 g of 4-(2-butynyloxy)-6-(3,3-dimethylpyrrolidin-1-yl)pyrimidine (hereinafter, referred to as Compound (27)).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07928110B2uspto-grants-2011_04