Réaction #1095866

ord-e8bc12bbbf184449afb3ff170682ebb5

Conditions de réaction

Température
57.5°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

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

Mode opératoire

Into 2 ml of N,N-dimethylformamide was resolved 183 mg of 4-chloro-6-(2-butynyloxy)pyrimidine, 166 mg of potassium carbonate and 71 mg of pyrrolidine was added therein, and the mixture was stirred for 4 hours at 55-60° 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 170 mg of 4-(2-butynyloxy)-6-(1-pyrrolidinyl)pyrimidine (hereinafter, referred to as Compound (17)).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07973028B2uspto-grants-2011_07