Реакция #1095866

ord-e8bc12bbbf184449afb3ff170682ebb5

Растворители

Условия реакции

Температура
57.5°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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)).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07973028B2uspto-grants-2011_07