Реакция #1179856

ord-d8715375c8804bc6a832e0f15e5c09b9

Растворители

Условия реакции

Температура
80°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 4 ml of N,N-dimethylformamide was resolved 0.36 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine, 0.62 g of potassium carbonate and 0.25 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 0.15 g of 4-(2-butynyloxy)-5-fluoro-6-(3,3-dimethylpyrrolidin-1-yl)pyrimidine (hereinafter, referred to as Compound (28)).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08129526B2uspto-grants-2012_03